DEPARTMENTAL IMS MANUAL

QUALITY CONTROL LABORATORY

COPY NO. : 1

ISSUE No. 01

EFFECTIVE DATE : 25/05/12

DESIGNATION : CHIEF MANAGER

DEPARTMENT : QUALITY CONTROL LABORATORY

CONTROLLED COPY UNCONTROLLED COPY

ISSUED BY : SECTIONAL HEAD SIGN:

(QUALITY CONTROL LAB.)

APPROVED BY : DEPARTMENTAL HEAD SIGN:

(QUALITY CONTROL LAB.)

RASHTRIYA CHEMICALS & FERTILIZERS LTD.

THAL UNIT,
TAL. : ALIBAG,
DIST.: RAIGAD.
PIN : 402 209
 ISO 9001:2000,
ISO-14001:2004,
OHSAS-18001:2007
ISSUE No: 01 REVISION No: 02
EFFECTIVE DATE: 20/10/13

CONTROLLED COPY
UNCONTROLLED COPY

I ISSUED BY: SECTIONAL HEAD (QUALITY CONTROL LAB.)

SIGN: _____________

APPROVED BY: DEPARTMENTAL HEAD (QUALITY CONTROL LAB.)

SIGN: __________________

RASHTRIYA CHEMICALS & FERTILIZERS LTD.

THAL UNIT, PIN: 402 208, TAL: ALIBAG, DIST: RAIGAD.
PHONE NO: 952141-238068 FAX NO.: 952141-238206.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: MASTER LIST OF DOCUMENTS

ISO 9001 -
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SETIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

Sr.No TITLE OF THE DOCUMENT COPY STATUS

DOCUMENT No.
. NO REV DATE

01 LABORATORY IMS MANUAL DM/QCLAB 02 00 25/05/12

HEAD QUALITY CONTROL LAB.

 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY

COPY NO. : 1

ISSUE No. 01

EFFECTIVE DATE : 25/05/12

DESIGNATION : CHIEF MANAGER

DEPARTMENT : QUALITY CONTROL LABORATORY

CONTROLLED COPY UNCONTROLLED COPY

ISSUED BY : SECTIONAL HEAD SIGN:

(QUALITY CONTROL LAB.)

APPROVED BY : DEPARTMENTAL HEAD SIGN:

(QUALITY CONTROL LAB.)

RASHTRIYA CHEMICALS & FERTILIZERS LTD.

THAL UNIT,
TAL. : ALIBAG,
DIST.: RAIGAD.
PIN : 402 209
 ISO 9001:2000,
ISO-14001:2004,
OHSAS-18001:2007
ISSUE No: 01 REVISION No: 01
EFFECTIVE DATE: 25/05/12

CONTROLLED COPY
UNCONTROLLED COPY

I ISSUED BY: SECTIONAL HEAD (QUALITY CONTROL LAB.)

SIGN: _____________

APPROVED BY: DEPARTMENTAL HEAD (QUALITY CONTROL LAB.)

SIGN: __________________

RASHTRIYA CHEMICALS & FERTILIZERS LTD.

THAL UNIT, PIN: 402 208, TAL: ALIBAG, DIST: RAIGAD.
PHONE NO: 952141-238068 FAX NO.: 952141-238206.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: MASTER LIST OF DOCUMENTS

ISO 9001 -
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SETIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

Sr.No TITLE OF THE DOCUMENT COPY STATUS

DOCUMENT No.
. NO REV DATE

01 LABORATORY IMS MANUAL DM/QCLAB 02 00 25/05/12

HEAD QUALITY CONTROL LAB.

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: LIST OF DOCUMENTS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 06
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

LIST OF DOCUMENTS

SR. TITLE OF THE DOCUMENT ISSUE NO. / EFFECTIVE

NO. REVISION NO. DATE

LABORATORY IMS MANUAL

PROCEDURES AND SPECIFICATIONS
01

WORK INSTRUCTIONS 01 / 06 25/05/12

FORMS AND FORMATS

LIST OF EXTERNAL ORIGIN.

HEAD QUALITY CONTROL LAB.

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: INDEX
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 2
PREPARED BY: SECTIONAL HEAD DATE:10.05.16
APPROVED BY: HOD

PAGE ISSUE / DATE OF

Sr. DOC.NO TITLE
NO. REV.NO REVISION

1 TH-IMS-QCL-DOC-01 INDEX 1 OF 2 - 10.05.16

2 TH-IMS-QCL-DOC-02 AUTHORISATION 1 OF 1 1/ 1 25.05.12

3 TH-IMS-QCL-DOC-03 INTRODUCTION TO MANUAL 1OF 1 1/ 0 25.03.08

4 TH-IMS-QCL-DOC-04 LIST OF COPY HOLDERS 1 OF 1 1/ 3 27.05.14

5 TH-IMS-QCL-DOC-05 PROFILE OF THE DEPARTMENT 1 OF 2 1/ 3 02.06.15

ABBREVATION AND
6 TH-IMS-QCL-DOC-06 DEFINATIONS
1 OF 3 1/2 27.05.14

7 TH-IMS-QCL-DOC-07 LIST OF RECORDS 1 OF 3 1/ 2 10.05.16

8 TH-IMS-QCL-ASP-14 ASPECT REGISTER 1 OF 1 2/0 10.05.16
9 TH-IMS-QCL-HRC-01 HIRA 1 OF 4 2/0 10.05.16
10 TH-IMS-QCL-D-PRC-01 RAW MATERIALS TESTING 1 OF 1 1/ 2 08.02.16

11 TH-IMS-QCL-D-PRC-02 PROCESS AND FINISHED

1 0F 1 1/ 3 01.12.15
PRODUCT ANALYSIS
12 TH-IMS-QCL-D-PRC-03 INSTRUMENTS CALIBRATION 1 OF 2 1/ 4 10.05.16
27.05.14
13 TH-IMS-QCL-D-PRC-04 CUSTOMER COMPLAINT 1 OF 1 1/ 2

10.05.16
14 TH-IMS-QCL-D-PRC-05 OUT SOURCE PROCESS 1 OF 1 1/ 4

10.05.16
15 TH-IMS-QCL-D-PRC-06 Legal Requirements 1 OF 1 1/0

SPECIFICATIONS OF RAW
16 TH-IMS-QCL-SPEC-01 MATERIAL AND PRODUCTS.
1 OF 13 1/2 10.05.16

17 TH-IMS-QCL-WRK-01 TESTING OF RAW MATERIAL 1 OF 20 1/1 10.05.16

ANALYSIS OF PROCESS
18 TH-IMS-QCL-WRK-02 SAMPLES, FINISHED PRODUCT.
1 OF 34 1/3 10.05.16

CALIBRATION OF LAB
19 TH-IMS-QCL-WRK-03 INSTRUMENTS
1 OF 7 1/ 2 01.12.12

PREPARATION OF
20 TH-IMS-QCL-WRK-04 LABORATORY REAGENTS
1 OF 13 1/ 1 25.0512

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: INDEX
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 2
PREPARED BY: SECTIONAL HEAD DATE:10.05.16
APPROVED BY: HOD

PAGES ISSUE / DATE OF

Sr. DOC.NO TITLE
NO. REV.NO REVISION

LOADING AND UNLOADING,

19 TH-IMS-OHS-WRK-01 STORAGE & USE OF GAS 1 OF 1 1/1 01.12.12
CYLINDER.

MOISTURE IN AMMONIA AND

20 TH-IMS-OHS-WRK-02 AMIDE SAMPLING AND 1 OF 1 1/1 01.12.12
ANALYSIS.

21 TH-IMS-OHS-WRK-03 SAMPLING. 1 OF 2 1/2 20.10.13

22 TH-IMS-QCL-SPLPT LIST OF SAMPLE POINTS 1 OF 3 1/ 2 25.05.12

23 TH-IMS-QCL-FREQ FREQUENCY OF SAMPLING 1 OF 4 1/2 01.04.13

24 TH-IMS-QCL-FORMAT FORMATS 1 OF 50 1/ 3 10.05.16

LIST OF DOC. OF EXTERNAL

25 TH-IMS-QCL-EXTOR 1 OF 3 1/ 3 10.05.16
ORIGIN

2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: AUTHORISATION
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-02
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.12

THE MANAGEMENT OF RASHTRIYA CHEMICALS & FERTILIZERS AUTHORISES THE

USE OF INTEGRATED MANAGEMENT SYSTEM AS DETAILED IN THIS MANUAL, FOR
QUALITY CONTROL LABORATORY LOCATED IN TECHNICAL BUILDING AND
RESPECTIVE PLANT LABORATORIES.
THE SECTIONAL HEADS LISTED IN THE DEPARTMENT PROFILE WILL ENSURE THE
EFFECTIVE IMPLEMENTATIONS OF THE SYSTEM AT ALL LEVELS.

HEAD QUALITY CONTROL LAB

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: INTRODUCTION TO MANUAL
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-03
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SECTINAL HEAD ISSUE NO: 01 REVISION NO: 00
APPROVED BY: HOD EFFECTIVE DATE: 25.03.2008

THIS IMS MANUAL HAS BEEN PREPARED BY SECTIONAL HEAD WITH A VIEW TO
PROVIDE GUIDELINES FOR MANAGEMENT OF INTEGRATED MANAGEMENT SYSTEM IN
ALL LABORATORIES. THE MANUAL WILL BE REVISED AS AND WHEN REQUIRED BY
CHANGEING ITS EXISTING PROCEDURES AND WORKING METHODS FOR CONTINUAL
IMPROVEMENT AND CUSTOMER SATISFACTION.
ALL PERSONNEL OF LABORATORIES ARE RESPONSIBLE FOR ADHERING TO
INTEGRATED MANAGEMENT SYSTEM OUTLINED IN THIS MANUAL.

HEAD QUALITY CONTROL LAB

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: LIST OF COPY HOLDERS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 OF 1
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 05.11.09

IMS IS A CONTROLLED DOCUMENT AND ITS COPIES ARE AVAILABLE WITH THE

FOLLOWING DEPARTMENTAL / SECTIONAL HEADS.

COPY NO. COPY HOLDER INITIALS ON RECEIPT

01 MASTER COPY WITH M.R.

02 HEAD (QUALITY CONTROL LAB.)

 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PROFILE OF THE DEPARTMENT
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-05
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 2
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 02.06.2015

Central chemical laboratory, along with water treatment laboratory was established in 1984
and started activities of analysis of raw material, process samples & finished products. There
after Heavy water laboratory was established in 1986 & Chemical Group laboratory in 1989.
The laboratory analysis is mainly divided into wet analysis and instrumental analysis. The wet
analysis includes analysis of cooling water, boiler water, process samples, finished products,
raw material etc. The instrumental analysis uses the sophisticated instruments like Gas
chromatograph, Density meter, Mass spectrometer, UV/visible spectrophotometer, Karl
Fischer titrator, FTIR, Sulphur analyzer, Tensile Testing machine etc.
The laboratory has following organizational structure.

DGM
(Quality Control Lab)

CHIEF MANAGER
(Quality Control Lab)

Sectional Head Sectional Head Sectional Head Sectional Head

WTP Lab Chem. Gr. Lab HWP Lab Central & ETP Lab

Sr. Manager/ Manager / Dy. Manager / Senior Eng./ Chemist ( officer)

Chemist

Operator cum Tech.

Mazdoor 1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PROFILE OF THE DEPARTMENT
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-05
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 2
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 02.06.2015

Roles and Responsibilities.

DGM ( QC Lab.):
• Co-ordination of laboratory activities for quality assurance.
• Communication from Top Management to C.M. lab./ all staff.
Chief Manager:
• Co-ordination of laboratory activities for quality assurance.
• Communication from Top Management to respective lab. staff.
Sr. Manager:
• Keep Co-ordination / feed back with concerned plants.
Manager :
Keep Co-ordination / feed back with concerned plants
• Analysis of specific samples.
• Report the results to plant personals after analysis.
• Generating and maintaining required reports / documents.
Dy. Manager:
• Keep Co-ordination / feed back with concerned plants.
• Analysis of specific samples.
• Report the results to plant personals after analysis.
• Generating and maintaining required reports / documents.
Senior Engg. :
• Routine analysis
• Generate analytical reports.
• Sampling of gas and specific samples.
Chemist ( officer gr.) :
• Routine analysis
• Generate analytical reports.
• Sampling of gas and specific samples.
Operator cum Tech. :
• Bag analysis
Mazdoor:
• General house keeping.
• Sampling and its preservation or disposal
• Reporting to Dy. Chief Chemist / Chief Chemist.

2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PROFILE OF THE DEPARTMENT
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-05
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 2
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 02.06.2015

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ABBREVIATIONS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-06
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 3
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

ABBREVIATIONS DESCRIPTION

IA INSTRUMENT AIR
UMHOS MICROMHOS
NTU NEPHLOMETRIC TURBIDITY UNIT
M-ALK METHYL ORANGE ALKALINITY
LIT. LITERS
MIN. MINIMUM
MAX MAXIMUM
MEOH METHANOL
MAP-P METHYLAMINE PLANT – PRODUCTION DEPARTMENT
MMA MONO METHYLAMINE
OK OKAY
OFF.SPEC. OFF SPECIFICATIONS
PROD. PRODUCTION
PR PROCEDURE
PM PLANT MANAGER
% PERCENTAGE
PPM PARTS PER MILLION
PG PRESSURE GAUGE
RI REFRACTIVE INDEX
REV REVISION
SOLN. SOLUTION
TMA TRIMETHYLAMINE
WRK WORK INSTRUCTION
WT WEIGHT
BR BURETTE READING
MAT. NO. MATERIAL NUMBER
1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ABBREVIATIONS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-06
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 3
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

ABBREVIATIONS DESCRIPTION
APHA AMERICAN PUBLIC HEALTH ASSOCIATION
KF KARL FISHER
N NORMALITY
GC GAS CHROMATOGRAPH
UV ULTRA VIOLET
FID FLAME IONIZATION DETECTOR
TCD THERMAL CONDUCTIVITY DETECTOR
AAT ADVANCED AMINE TECHNOLOGIES
EDTA ETHYL DIAMINE TETRA ACETIC ACID
NAOH SODIUM HYDROXIDE
NH4CL AMMONIUM CHLORIDE
KNH2 POTASSIUM AMIDE
H2SO4 SULFURIC ACID
HNO3 NITRIC ACID
CM CENTIMETER
CH3COOH ACETIC ACID
KSCN POTASSIUM THIOCYNATE
FE IRON
AGNO3 SILVER NITRATE
HCL HYDROCHLORIC ACID
NH4BR AMMONIUM BROMIDE
NA2S2O3 SODIUM THIOSULPHATE
NH3 AMMONIA
E.B.T. ERICHROME BLACK T
M.O. METHYL ORANGE
2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ABBREVIATIONS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-06
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 3
PREPARED BY: SECTIONAL HEADS ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

ABBREVIATIONS DESCRIPTION
µ MICRO
ºC DEGREE CENTIGRADE
R.T. ROOM TEMPERATURE
↑ EVOLUTION OF GAS
PRO PRIMARY REFORMER OUTLET
HTI HIGH TEMPERATURE INLET
HTO HIGH TEMPERATURE CO CONVERTOR
MTO MEDIUM TEMPERATURE CO CONVERTOR
LTO LOW TEMPERATURE CO CONVERTOR
ABO ABSORBER OUTLET
METHO METHANATOR OUTLET
S-200 IN S- 200 INLET
S-200 OUT S-200 OUTLET
S-50 OUT S-50 OUTLET
FA FORMIC ACID
NG NATURAL GAS
RLNG RELIANCE NATURAL GAS

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: LIST OF RECORDS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-07
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

SR REV. STORING DETAILS

DOCUMENT NO. TITLE
NO NO.
LOCATION PERIOD
TH-IMS-FR/ QCL-CL GENERAL SHIFT REPORT CENTRAL
1 ( CENTRAL LAB) 02 4 YEARS
/01-A,B,C,D,E,F,G,H, LAB.
TH-IMS-FR/ QCL-CL SHIFT ANALYSIS REPORT CENTRAL
2 02 4 YEARS
/02- A, B CENTRAL LAB. LAB.
TH-IMS-FR/ QCL-CGL RAW MATERIAL ( C.G.P)
4 00 C.G.P.LAB. 4 YEARS
/01 & 03
ANALYSIS OF COOLING
TH-IMS-FR/ QCL-CGL
5 WATER & FINISHED 00 C.G.P.LAB. 4 YEARS
/05
PRODUCTS.
SHIFT ANALYSIS
TH-IMS-FR/ QCL-CGL RECORD A- Amines (old &
6 00 C.G.P.LAB. 4 YEARS
/06, A,B & C. new) & B- DMF & DMAC &
C – FORMIC ACID
7 TH-IMS-FR/ QCL-CGL LAB. DISPATCH
00 CGP LAB. 4 YEARS
/07 TO 10 CERTIFICATES
TH-IMS-FR/ QCL-CGL STASTICAL RECORD FOR
8 00 CGP LAB. 4 YEARS
/11 TO 14 PRODUCT BATCH TANKS.
TH-IMS-FR/ QCL-HWL SHIFT ANALYSIS
9 01 HWP LAB. 4 YEARS
/01 RECORD. ( HWP)
TH-IMS-FR/ QCL-HWL
10 DAILY REPORT ( HWP ) 01 HWP LAB. 4 YEARS
/02
13 TH-IMS-FR/ QCL- SHIFT ANALYSIS REPORT
00 WTP LAB 4 YEARS
WTPL /01 ( I,II,III) W.T.P. LAB.
TH-IMS-FR/ QCL- GENERAL SHIFT REPORT
14 00 WTP LAB 4 YEARS
WTPL /02 WTP LAB.
TH-IMS-FR/ QCL- ANALYSIS REPORT OF
15 00 WTP LAB 4 YEARS
WTPL /03 MIDC WATER WTP LAB.
TH-IMS-FR/ QCL- RAW MATERIAL REPORT
16 01 WTP LAB 4 YEARS
WTPL /04 TO 09 WTP
TH-IMS-FR/ CCL- ETPL GENERAL SHIFT REPORT
17 00 ETP LAB. 4 YEARS
/01 ETP

GENERAL SHIFT REPORT 4 YEARS

TH-IMS-FR/ CCL- ETPL
18 ETP 00 ETP LAB
/02
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: LIST OF RECORDS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-07
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

SR REV. STORING DETAILS

DOCUMENT NO. TITLE
NO NO.
LOCATION PERIOD
TH-IMS-FR/ CCL- ETPL GENERAL SHIFT REPORT
19 00 ETP.LAB. 4 YEARS
/03 ETP
RECORDS FOR
ALL
20 TH-IMS-REC/ QCL /01 INSTRUMENTS 00 4 YEARS
LABS.
CALIBRATION.
RECORDS FOR
TH-IMS-REC/ QCL /02- CENTRAL
21 CUSTOMER COMPLAINT 00 4 YEARS
A LAB.
REGISTER.
CUSTOMER COMPLAINT
TH-IMS-REC/ QCL /02- CENTRAL
22 CORRESPONDENCE 00 4 YEARS
B LAB
RECORDS FOR CENTRAL
23 TH-IMS-REC/ QCL /03 00 4 YEARS
OBJECTIVES. LAB
BAG LOT ENTRY CENTRAL
24 TH-IMS-REC/ QCL /04 00 4 YEARS
REGISTER LAB
RAW MATERIAL
25 TH-IMS-REC/ QCL /05 00 WTP LAB 4 YEARS
REGISTER
IMS POLICY & CENTRAL
26 TH-IMS-REC/ QCL /06 00 4 YEARS
LOCATIONS LAB
CORE GROUP MEETING
CENTRAL
27 TH-IMS-REC/ QCL /07 RECORD 00 4 YEARS
LAB.
MANAGEMET REVIEW
CENTRAL
28 TH-IMS-REC/ QCL /08 MEETING RECORD 00 4 YEARS
LAB
RECORD OF
DEPARTMENTAL CENTRAL
29 TH-IMS-REC/ QCL /09 00 4 YEARS
MEETING LAB

HAZARD
IDDENTIFICATION CENTRAL
30 TH-IMS-REC/ QCL /10 00 4 YEARS
REGISTER LAB.

TRAINING RECORD CENTRAL

31 TH-IMS-REC/ QCL /11 00 4 YEARS
LAB
TRAINING NEEDS & CENTRAL
32 TH-IMS-REC/ QCL /12 00 4 YEARS
COMPETENCY MATRICS LAB
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: LIST OF RECORDS
ISO 9001 - DOC.NO: TH-IMS-QCL-DOC-07
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

IMS MANAGEMENT PLAN CENTRAL

33 TH-IMS-REC/ QCL /13 00 4 YEARS
LAB
OPERATIONAL
CENTRAL
34 TH-IMS-REC/ QCL /14 CONTROL PROCEDURE 00 4 YEARS
LAB
EMERGENCY
CENTRAL
35 TH-IMS-REC/ QCL /15 PREPAREDNESS PLAN 00 4 YEARS
LAB.
MOCK DRILL CENTRAL
36 TH-IMS-REC/ QCL /16 00 4 YEARS
LAB
STATISTICAL RECORD CENTRAL
37 TH-IMS-REC/ QCL /17 00 4 YEARS
LAB
IMS AUDIT, NC/ OBS./ATR CENTRAL
38 TH-IMS-REC/ QCL /18 00 4 YEARS
LAB.
OBSOLETE DOCUMENTS CENTRAL
39 TH-IMS-REC/ QCL /19 00 4 YEARS
LAB
CENTRAL
40 TH-IMS-REC/ QCL /20 OUTSOURCE PROCESS 00 4 YEARS
LAB
CENTRAL
41 TH-IMS-REC/ QCL /21 NEW METHOD FILE 00 4 YEARS
LAB
TH-IMS-REC/ QCL /22 NEEM OIL TESTING CENTRAL
42 00 4 YEARS
A&B RECORD LAB
CENTRAL
43 TH-IMS-REC/ QCL /23 MORNING MEETING FILE 00 4 YEARS
LAB
CENTRAL
44 TH-IMS-4-ASP-14 ASPECT REGISTER 02/00 4 YEARS
LAB
CENTRAL
45 TH-IMS-QCL-HRC-01 HIRA 02/00 4 YEARS
LAB
CENTRAL
46 TH-IMS-QCL-REC-24 Work Monitoring Record 00 4 YEARS
LAB
 Document no. TH-IMS-QCL-HRC-01
INTEGRATED MANAGEMENT SYSTEM
Title : Hazard Identification and Risk Assesment (HIRA) Page 4 of 4
OHSAS-18001 : 2007 Clause : 4.3.1 Issue No. 02
Revision No 00
Effective Date 10.05.2016
APPROVED BY Released by

Designation Chief Manager Designation Sectional Head (lab)

Plant/Department Quality control lab
Risk Assesment Risk Level
Risk Control Remarks
R/
Refer annexure V Process Residual Legal
Sr. NR Risk category
Activity Hazard Existing Control & PPE'S WRK/SMP/OCP Risk (Y/N)
No /E
Severity Probability ( proposed
M AXB
(A) (B) control)
For specific health hazards due to toxic chemicals,refer the chemical hazards table in Annexure I, For Physical health hazards like High /Low temperature,vibrations,noise,ergonomics & electrical, refer the physical hazards table in
Annexure II, For specific PPE's to be used, refer Annexure III & For existing controls, refer Annexure IV.

HIRA risk matrix : 1-6 (Trivial),8-10 (Acceptable),12-18 (Moderate),20-24 (Substantial),25-30(Very Substantial),36 (Intolerable)
“Behavioural related hazards such as memory limitations, information processing problems, distraction, fatigue, visual activity limitations, decision-making biased by experience and knowledge, rigid problem solving, susceptibility
to following group behaviour etc, have been considered in HIRA”.
1.0 Loading,Transporation Unloading,Storage,Use of
Irritation to Nose,Eye,Skin & respiratory TH-IMS-QCL-EMP-01,02,10, TH-IMS-QCL-
S3,4,
1.1 Chemicals R tract,Flashing on body during handling of 2 2 4 None 4 N Trivial OCP-02,TH-IMS-6-QCL-SMP-01,10 TH-IMS-
PPE :P6,P19,P24
chemicals. REC-QCL-24
S3,S4,
1.2 Glassware R Skin Cuts during handling glassware 3 2 6 None 6 N Trivial
PPE: P15,P19
Hydrogen,nitrogen,Oxyg Leakage,Bursting of cylinder,Burn, Asphyxia S7 TH-IMS-OHS-L-WRK-01, TH-EMS-6--EMP-121,TH-IMS-QCL-SMP-
1.3 NR 4 2 8 None 4 Y Trivial
en,Argon, LPG Cylinder during handling of cylinders TH-OHSAS-QCL-OCP-1 03/04/06, TH-IMS-QCL-OCP-05

S3,S4,
Health hazards due to exposure to carbon di-
1.4 Dry ice R PPE: P15,P19 3 1 3 None 3 N Trivial TH-IMS-QCL-EMP-06
oxide gas,cold Burn, Asphyxia
TH-IMS-OHS-L-WRK-03
S3,S4
1.5 Liquid Air NR Cold Burn, Flashing on body PPE :P19,P24 4 1 4 None 4 N Trivial TH-IMS-6-QCL-SMP-01
TH-IMS-OHS-L-WRK-03

1.6 Hydrogen Generator R Over pressure S2,S3,S4,S7 3 1 3 None 3 N Trivial TH-IMS-QCL-OCP-03

2.0 Sampling
2.1 Raw Material

Fall from hight, irritation to Nose,Eye,Skin &

Tanker Samples (Acid / respiratory tract,Flashing on body, S3,S4,PPE : P6, P26,P24 TH-
2.1.1 R 4 2 8 None 8 N Acceptable TH-IMS-6-QCL-SMP-01
Alkali / Methanol) Acid/alkali burn, skin absorption of methanol IMS-OHS-L-WRK-03
may results in sickness & fire

Cooling water & other Irritation to Nose,Eye,Skin & respiratory TH-IMS-REC-QCL-24,TH-IMS-QCL-OCP-

2.1.2 R S3,S4 PPE : P6,P26, P11,P24 4 1 4 None 4 N Trivial
allied chemicals tract,Flashing on body 02,TH-IMS-QCL-SMP-10
 Document no. TH-IMS-QCL-HRC-01
INTEGRATED MANAGEMENT SYSTEM
Title : Hazard Identification and Risk Assesment (HIRA) Page 4 of 4
OHSAS-18001 : 2007 Clause : 4.3.1 Issue No. 02
Revision No 00
Effective Date 10.05.2016
APPROVED BY Released by

Designation Chief Manager Designation Sectional Head (lab)

Plant/Department Quality control lab
Risk Assesment Risk Level
Risk Control Remarks
R/
Refer annexure V Process Residual Legal
Sr. NR Risk category
Activity Hazard Existing Control & PPE'S WRK/SMP/OCP Risk (Y/N)
No /E
Severity Probability ( proposed
M AXB
(A) (B) control)
For specific health hazards due to toxic chemicals,refer the chemical hazards table in Annexure I, For Physical health hazards like High /Low temperature,vibrations,noise,ergonomics & electrical, refer the physical hazards table in
Annexure II, For specific PPE's to be used, refer Annexure III & For existing controls, refer Annexure IV.

HIRA risk matrix : 1-6 (Trivial),8-10 (Acceptable),12-18 (Moderate),20-24 (Substantial),25-30(Very Substantial),36 (Intolerable)
“Behavioural related hazards such as memory limitations, information processing problems, distraction, fatigue, visual activity limitations, decision-making biased by experience and knowledge, rigid problem solving, susceptibility
to following group behaviour etc, have been considered in HIRA”.
2.2 In process & Finshed Product

Hot water condensate, Physical or burn injury due to release of hot S3,S4 PPE: P15,P26,P11 TH-
2.2.1 R 4 2 8 None 8 N Acceptable TH-EMS-6--EMP-09
Boiler water condensate IMS-OHS-L-WRK-03

Physical or burn injury due to release of hot

Reactor/ Stripper (water S3,S4PPE: P15,P26,P11 TH-
2.2.2 R condensate ,Irritation to Nose,Eye,Skin & 2 2 4 None 4 N Trivial
samples) IMS-OHS-L-WRK-03
respiratory tract,Flashing on body

Physical or burn injury due to release of hot

S3,S4PPE: P15,P26,P11 TH-
2.2.3 Effluent water R condensate ,Irritation to Nose,Eye,Skin & 2 2 4 None 4 N Trivial
IMS-OHS-L-WRK-03
respiratory tract,Flashing on body

Physical or burn injury due to release of hot

S3,S4PPE: P15,P26,P11 TH- TH-IMS-QCL-EMP-02,TH-IMS-QCL-SMP-
2.2.4 GV / MEA solution R condensate ,Irritation to Nose,Eye,Skin & 4 2 8 None 8 N Acceptable
IMS-OHS-L-WRK-03 01,TH-IMS-REC-QCL-24
respiratory tract,Flashing on body

Anhydrous ammonia / S3,S4,

Irritation to Nose,Eye,Skin & respiratory TH-IMS-QCL-EMP-04,TH-IMS-QCL-SMP-
2.2.5 Amide solution in R PPE : P19,P11,P26,P24 TH- 3 2 6 None 6 N Acceptable
tract,Frost bit,Flashing on body & fire. 01,TH-IMS-REC-QCL-24
ammonia IMS-OHS-L-WRK-02

S3,S4
Irritation to Nose,Eye,Skin & respiratory TH-IMS-6-QCL-SMP-01,TH-IMS-REC-QCL-
2.2.6 DMF,DMAc & MA Plant R PPE : P19,P11,P26,P24 TH- 4 2 8 None 8 N Acceptable
tract,Flashing on body 24
IMS-OHS-L-WRK-03

S3,S4 PPE
Irritation to Nose,Eye,Skin & respiratory TH-IMS-6-QCL-SMP-01,TH-IMS-REC-QCL-
2.2.7 Formic acid plant R : P19,P11,P26,P24 TH-IMS- 4 2 8 None 8 N Acceptable
tract,Acid burn,Flashing on body 24
OHS-L-WRK-03

S3,S4
2.3 Vessle Entry Sample NR Irritation to Nose,Eye,Skin & respiratory tract 3 1 3 None 3 N Trivial TH-IMS-6-QCL-SMP-01 &07
PPE : P19,P11,P26,P24, P27

S3,S4,PPE:P12,P26,P24,P27,T
2.4 sampling at height R Fall from hight, 6 2 12 none 12 N significant
H-IMS-OHS-L-WRK-03,
 Document no. TH-IMS-QCL-HRC-01
INTEGRATED MANAGEMENT SYSTEM
Title : Hazard Identification and Risk Assesment (HIRA) Page 4 of 4
OHSAS-18001 : 2007 Clause : 4.3.1 Issue No. 02
Revision No 00
Effective Date 10.05.2016
APPROVED BY Released by

Designation Chief Manager Designation Sectional Head (lab)

Plant/Department Quality control lab
Risk Assesment Risk Level
Risk Control Remarks
R/
Refer annexure V Process Residual Legal
Sr. NR Risk category
Activity Hazard Existing Control & PPE'S WRK/SMP/OCP Risk (Y/N)
No /E
Severity Probability ( proposed
M AXB
(A) (B) control)
For specific health hazards due to toxic chemicals,refer the chemical hazards table in Annexure I, For Physical health hazards like High /Low temperature,vibrations,noise,ergonomics & electrical, refer the physical hazards table in
Annexure II, For specific PPE's to be used, refer Annexure III & For existing controls, refer Annexure IV.

HIRA risk matrix : 1-6 (Trivial),8-10 (Acceptable),12-18 (Moderate),20-24 (Substantial),25-30(Very Substantial),36 (Intolerable)
“Behavioural related hazards such as memory limitations, information processing problems, distraction, fatigue, visual activity limitations, decision-making biased by experience and knowledge, rigid problem solving, susceptibility
to following group behaviour etc, have been considered in HIRA”.
3.0 Analysis
3.1 Chemical Analysis
PPE : P19,P11,P26,P24, P27,
Irritation to Nose,Eye,Skin & respiratory TH-IMS-QCL-EMP-02, TH-IMS-6-QCL-SMP-
3.1.1 Raw Material Analysis R Apron,Fume Hood Safety 4 1 4 None 4 N Trivial
tract,Flashing on body 01,10,TH-IMS-REC-QCL-24
Shower.

Irritation to Nose,Eye,Skin & respiratory S3,S4 PPE : P19,P11,P26,P24, TH-IMS-QCL-EMP-04,TH-IMS-6-QCL-SMP-

3.1.2 Moisture in ammonia R 3 2 6 None 6 N Acceptable
tract,Flashing on body, Potassium metal fire P27 TH-IMS-OHS-L-WRK-03 01 & 10,TH-IMS-REC-QCL-24

PPE : P19,P11,P26,P24, P27, TH-IMS-QCL-EMP-01,TH-IMS-QCL-OCP-

Irritation to Nose,Eye,Skin & respiratory
3.1.3 GV / MEA solution R Apron,Fume Hood Safety 3 2 6 None 6 N Trivial 02,TH-IMS-6-QCL-SMP-10, TH-IMS-REC-
tract,Flashing on body
Shower. QCL-24
Ammonia in sythesis S3,S4
3.1.4 R Irritation to Nose,Eye,Skin & respiratory tract 3 2 6 None 6 N Trivial
gas PPE:P4
PPE : P19,P11,P26,P24, P27,
Irritation to Nose,Eye,Skin & respiratory
3.1.5 Reactor/ Stripper R Apron,Fume Hood Safety 3 2 6 None 6 N Trivial
tract,Flashing on body
Shower.
3.2 Instrumental analysis
While cutting bags by scissor finger may got S3,S4
3.2.1 HDPE/Jute bag R 3 2 6 None 6 N Trivial
cut PPE:P16
S3,S4,S16
3.2.2 Gas Chromatography R Burn due to fire, Asphyxia 4 2 8 None 8 N Acceptable
PPE:P4,P16,P26
S3,S4,S16 TH-IMS-6-QCL-SMP-01,TH-IMS-QCL-EMP-
3.2.3 Mass spectrometer R Elecrtical shock & Burn due to fire 3 2 6 None 6 N Trivial
PPE:P4,P16,P26 05
Irritation to Nose,Eye,Skin & respiratory
S3,S4,S16
3.2.4 Laboratory Cracker R tract,Flashing on body, electrical shock & 3 2 6 None 6 N Trivial
PPE:P4,P16,P26
fire

S3,S4,S16
3.2.5 Flame photometer R Burn due to fire 3 2 6 None 6 N Trivial TH-IMS-QCL-SMP-01
PPE:P4,P16,P26
 Document no. TH-IMS-QCL-HRC-01
INTEGRATED MANAGEMENT SYSTEM
Title : Hazard Identification and Risk Assesment (HIRA) Page 4 of 4
OHSAS-18001 : 2007 Clause : 4.3.1 Issue No. 02
Revision No 00
Effective Date 10.05.2016
APPROVED BY Released by

Designation Chief Manager Designation Sectional Head (lab)

Plant/Department Quality control lab
Risk Assesment Risk Level
Risk Control Remarks
R/
Refer annexure V Process Residual Legal
Sr. NR Risk category
Activity Hazard Existing Control & PPE'S WRK/SMP/OCP Risk (Y/N)
No /E
Severity Probability ( proposed
M AXB
(A) (B) control)
For specific health hazards due to toxic chemicals,refer the chemical hazards table in Annexure I, For Physical health hazards like High /Low temperature,vibrations,noise,ergonomics & electrical, refer the physical hazards table in
Annexure II, For specific PPE's to be used, refer Annexure III & For existing controls, refer Annexure IV.

HIRA risk matrix : 1-6 (Trivial),8-10 (Acceptable),12-18 (Moderate),20-24 (Substantial),25-30(Very Substantial),36 (Intolerable)
“Behavioural related hazards such as memory limitations, information processing problems, distraction, fatigue, visual activity limitations, decision-making biased by experience and knowledge, rigid problem solving, susceptibility
to following group behaviour etc, have been considered in HIRA”.
S3,S4,S16
3.2.6 FTIR R IR radiation 3 2 6 None 6 N Trivial TH-IMS-QCL-SMP-01
PPE:P4,P16,P26
S3,S4,S16
3.2.7 Ovens R Hot burn,shock 2 1 2 None 2 N Trivial TH-IMS-QCL-EMP-05
PPE:P4,P16,P26

Irritation to Nose,Eye,Skin & respiratory S3,S4,S16

3.2.8 Sulfur Analyzer R 2 1 2 None 2 N Trivial
tract, Acid burn,hot burn PPE:P4,P16,P26
4.0 Disposal

4.1 Laboratory Effluent R Irritation to Nose,Eye,Skin & respiratory tract Fixed location,close drain 2 1 2 None 2 N Trivial Th-EMS-6-OCP-74

4.2 Unused Sample R Irritation to Nose,Eye,Skin & respiratory tract Fixed location,close Container 2 1 2 None 2 N Trivial Th-EMS-6-OCP-76
5.0 Utilities
S3,4,8,
Physical or body / burn injury due to
5.1 Electrical power R PPE:P1,3,11,15,26,27,30 3 2 6 None 6 N Trivial TH-IMS-QCL-EMP-06
electrical shock

6.0 Behavioural
Collection of Hazardous NR Behavioral Hazards Avoided during shift end (1
6.1 Hr) / change 1 3 3 None 3 N Trivial
samples
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Sampling procedure for polypropylene twine On the basis of IS 12734 : 2002

ISO 9001 - 7.5 DOC.NO: TH-IMS-QCL-D-

ISO 14001 - 4.4.6
OHSAS 18001 - 4.4.6 PAGE NO: 1 OF 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 00
APPROVED BY: HOD EFFECTIVE DATE: 20.02.2015

1. Definitions:

a. Lot: The quantity of boxes / packages containing polypropylene twine of the same construction
supplied to one buyer against one dispatch note.
b. Package / Box: Contains polypropylene twine spools.

2. Sampling procedure:

a. Draw the sample packages at random by using following formula,

S= 0.4 x N1/2
Where,
N= Total no. of packages in the lot; S = No. of packages to be selected
If “S” is not a whole number then round off the value as per IS 2:1960

b. From each package selected, draw at least five spools.

Sampling should be done as per table given below,

Sr. No of Packages Select No. of Draw No. of Spools

No. received packages( S )
1 01 to 13 1 5
2 14 to 37 2 10
3 38 to 74 3 15
4 75 to 120 4 20

Note: If “S” is less than 1, Select 1 package.

3. Conformity tests

a. Breaking strength and Percent Elongation ( IS: 1670)

• Cut two specimens from a spool and check their strength and elongation.
• Average of these two specimen test results shall be considered as breaking strength and
percent elongation for that spool only.
• Check all the sample spools for strength and Elongation.
• Calculate average breaking strength and percent elongation of all the sample spools.
• Consider this average for conformity of the lot.

b. Runnage ( m/kg )

• Check the runnage for spools with minimum and maximum breaking strength.
• Remove 25 meter length and weigh. From the mass compute the length in meter per
kilogram.

For conformity of the lot, test result of Breaking strength, % Elongation and runnage should satisfy
the specified value given in PO.

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: RAW MATERIAL TESTING

ISO 9001 - 7.5 DOC.NO: TH-IMS-QCL-D-PRC-01

ISO 14001 - 4.4.6
OHSAS 18001 - 4.4.6 PAGE NO: 1 OF 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 08.02.2016

OBJECTIVE : To ensure the raw and packaging material quality as per specification.
PURPOSE : To test the raw materials Quality.
SCOPE : To check the critical parameters of chemical and packaging materials supplied by
various suppliers and in process and finished products as per specifications.
RESPOSIBILITIES: FUNCTIONAL: Sectional head (lab)
OPERATIONAL: Dy. Manager, Manager and Chemist.
PROCEDURE:
1. In plant Raw material: Lab representative collects the sample as per schedule and plant
requirement.
2. Raw material from store: Store personals send sample along with concern documents to lab.
3. Packaging Material from PHP: Bagging personals send sample along with concern documents
to lab. Details are noted down with time in register.
4. Neem oil from PHP: Bagging personals send sample along with concern document to lab.
Details are noted down with time in register.
5. Tested samples of bags and neem oil are kept for period of 12 weeks at designated place.
6. Tested samples of thread are kept for period of 4 weeks at designated place.

INPUT: Routine sampling schedule and requirement from shift In-charge on telephone.

OUTPUT: Raw packaging material test reports, Packaging Material and Neem oil register

MEASUREMENTS: Purity and other parameters.

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY

TITLE: PROCESS AND FINISHED PRODUCT ANALYSIS

ISO 9001 - 7.5 DOC.NO: TH-IMS-QCL-D-PRC-02
ISO 14001 - 4.4.6
OHSAS 18001 - 4.4.6 PAGE NO: 1 of 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2015

OBJECTIVE: To check quality of process samples and finished products.

PURPOSE: To maintain product quality as per specifications.
SCOPE: To analyze various samples for critical parameters.
RESPONSIBILITIES: FUNCTIONAL : Sectional head (lab)
OPERATIONAL : Chief Chemist, Dy. Chief Chemist. Chemist
INPUT: Requisition for process samples, finished product and dispatched material from shift
In-charge as per schedule or as per requirement.
PROCEDURE:
Collect the sample by mazdoor, chemist or lab officers.
Analysis of samples by chemist/Lab officer. (QCL/WRK/02),
Report the analysis to shift In-charge on telephone.
Enter in appropriate formats and SAP system.
All unused samples are recycled or disposed off. Urea product sample preserved for 30 days.
For in plant product deviation, corrective measures are taken by the plant and sample is
reanalyzed.
REFERENCE DOCUMENTS: QCL/WRK/02.
OUTPUT: Analysis report.
MEASUREMENTS: Critical parameters as per requirement.
QUALITY RECORD: TH-IMS/TH-IMS/TH-IMS/TH-IMS/TH-IMS/FR/QCL-CL/01-A & B, TH-
IMS/TH-IMS/FR/QCL-CL/02, TH-IMS/FR/QCL-CGL/05, TH-IMS/FR/QCL-CGL/06 A, B and C, TH-
IMS/FR/QCL-HWL/01, TH-IMS/FR/QCL-WTL/01 and TH-IMS/FR/QCL-ETPL/01,

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: INSTRUMENTS CALIBRATION
ISO 9001 - 7.6 DOC.NO: TH-IMS-QCL-D-PRC-03
ISO 14001 -4.5.1
OHSAS 18001 -4.5.1 PAGE NO: 1 of 2
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 04
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

OBJECTIVE: Calibration of instruments.

PURPOSE: To maintain the accuracy of the analytical results.
SCOPE: Calibration of instruments in laboratories.
RESPONSIBILITIES: FUNCTIONAL: Sectional head (lab)
OPERATIONAL: Dy. /Chief Chemist, Chemist.
INPUT: Checking calibration with standards.
PROCEDURE DETAILS:
1. Check calibration date.
2. Prepare standard solutions as per QCL/WRK/04
3. Calibrate Instrument as per QCL/WRK/03.
4. Record data
5. Tag the instrument.
REFERENCE DOCUMENTS: QCL/WRK/03, REC/QCL/01.
OUTPUT: Calibration of instruments and data generated by calibration.
MEASUREMENT: Accuracy of instruments.
QUALITY RECORDS: TH-IMS/REC/QCL/01. (Central Lab., Chem.Gr.lab, H.W.P. Lab., W.T.P.
Lab., E.T.P.lab.)

Following instruments are calibrated once in two months.

pH meter

Conductivity meter

Karl-Fisher moisture analyzer

Nephelometer.

Karl fisher Titrino

Digital Burette

Refractometer

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: INSTRUMENTS CALIBRATION
ISO 9001 - 7.6 DOC.NO: TH-IMS-QCL-D-PRC-03
ISO 14001 -4.5.1
OHSAS 18001 -4.5.1 PAGE NO: 2 of 2
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 04
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Following instruments are calibrated once in six months.

UV-VIS Spectrophotometer

Gas chromatograph

Density meter

Mass spectrometer

FTIR

Foss Nitrogen analyzer

Viscosity meter is calibrated once in twelve month by in-house standard.

Tensile testing machine is calibrated once in twelve month by external agency.
Balances are calibrated quarterly by external agency.
Multi Gas detector is calibrated once in twelve month by external agency.

2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CUSTOMER COMPLAINT
ISO 9001 - 7.2.3 DOC.NO: TH-IMS-QCL-D-PRC-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

OBJECTIVE: To redress customer complaint.

PURPOSE: Satisfaction of customer.
SCOPE: For customer complaint, analyze the party sample or preserved counter
sample in laboratory or joint analysis at site or external parties works.
RESPONSIBILITIES: FUNCTIONAL: Sectional head (lab)
OPERATIONAL: Dy / Chief Chemist, Chemist.
INPUT: Customer complaint from Operation Manager.
PROCEDURE DETAILS:
Check preserved counter sample or jointly analyze at site or parties works for concerned test.
Analyze the same for deviating parameters. If it is within specifications, Give feed back to O.M.
If it is not within specs. Re analyze and Check calibration of instruments. If not O.K., then
standardize the same.
REFERENCE DOCUMENTS: QCL/WRK/02., QCL/WRK/03.
OUTPUT: Customer satisfaction.

MEASUREMENTS: Parameter of concerned test.

QUALITY RECORDS: TH-IMS/REC/QCL/02-A, TH-IMS/REC/QCL/02-B

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CUSTOMER COMPLAINT
ISO 9001 - 7.2.3 DOC.NO: TH-IMS-QCL-D-PRC-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 1
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 27.05.14

OBJECTIVE: To redress customer complaint.

PURPOSE: Satisfaction of customer.
SCOPE: For customer complaint, analyze the party sample or preserved counter sample
in laboratory or joint analysis at site or external parties works.

RESPONSIBILITIES: FUNCTIONAL: Sectional head (lab)

OPERATIONAL: Chemist, Chemist (Officer), Dy. Manager, Manager.
INPUT: Customer complaint from Operation Manager (OM).
PROCEDURE DETAILS:

• Complaints received from OM are taken up on highest priority by Chief Manager.

• On receiving of the complaint, Chief Manager reviews its nature.
• If complaint is related to test results, then preserved sample is retested with consent of OM.
• Retesting will be witnessed by the Chief Manager.
• If any discrepancy is not found in test results then informed OM.
• If any discrepancy is found in test results, an amendment test report will be issued.
• If there are reasons to believe that non-compliance with a certain aspect of the quality
system is suggested in the complaint, corrective and preventive actions are taken to
resolve the suggested complaint as well as to stop recurrence of such problem.
• All communication of complaint is routed through OM by Chief Manager.

REFERENCE DOCUMENTS: QCL/WRK/02., QCL/WRK/03.

OUTPUT: Customer satisfaction.

MEASUREMENTS: Parameter of concerned test.

QUALITY RECORDS: TH-IMS/REC/QCL/02-A, TH-IMS/REC/QCL/02-B

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Control of Outsourced Processes
ISO 9001 - 4.1 DOC.NO: TH-IMS-QCL-PRC-05
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 1
PREPARED BY: SETIONAL HEAD ISSUE NO: 01 REVISION NO: 04
APPROVED BY: HOD EFFECTIVE DATE: 10/05/16

1.0 PURPOSE:
This procedure is established to define the type and extent of control to be applied to the
outsourced processes carried out in quality control laboratory.

2.0 SCOPE:
Outsourced processes use in quality control laboratory.
3.0 RESPONSIBILITIES: Functional : CM (CC Lab)
Operational: Sectional heads

4.0 PROCEDURE:
4.1. The outsourced processes applicable to quality control laboratory identified are,
microbiological analysis and AMC of laboratory instruments.
4.2. Process control evaluation matrix for all these activities is available TH-IMS-
ES-D-DOC-01 in departmental IMS manual of engineering services.
4.3. Adequacy of existing control is reviewed after one year. If found inadequate
additional control shall be applied for out sourced processes.

Sr. Outsourced Potential Competence of Existing Proposed

No. Activity of Impact External Party Control Control
(PI) (if any)
1 AMC of Lab Major OEM’s Scope of -
Instrument * Recommendation work
2 Microbiological Major Company Scope of -
analysis Approved work

* List Of Laboratory Equipment’s covered under AMC.

Sr. No. Name of Instrument.
1 UV Spectrophotometer
2 Chemito GC
3 Karl fisher titrator
4 Bag testing machine
5 Deep Freezer
6 FTIR
7 Hydrogen Generator
8 Multi Gas Detector

5. 0 REFERENCE DOCUMENT:
1. TH-IMS-MGM-D-PRC-14 of system procedure manual.
2 TH-IMS-ES-D-DOC-01 in departmental IMS manual of ES.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Compliance of legal requirement
ISO 9001 - 7.2.1 DOC.NO: TH-IMS-QCL-PRC-06
ISO 14001 - 4.3.2
OHSAS 18001 - 4.3.2 PAGE NO: 1 of 1
PREPARED BY: SETIONAL HEAD ISSUE NO: 01 REVISION NO: 00
APPROVED BY: HOD EFFECTIVE DATE: 10/05/16

1.0 PURPOSE:
This procedure is established to comply the legal requirements applicable to quality control
laboratory.

2.0 SCOPE:
This procedure is applicable only for calibration of balances & weight box used
in quality control laboratory to comply legal requirement.

3.0 RESPONSIBILITIES: Functional : CM (CC Lab)

Operational: Sectional heads

4.0 PROCEDURE:
Refer OCP : TH-IMS-QCL-OCP-06
4.2 Ensure the balances are calibrated from external agency & in house
calibration as per requirement As per manual TH-IMS-QCL-WRK-03.
Ensure the weight box is sent to external agency for calibration.
Frequency of Balances calibration : quarterly
Frequency of weight box calibration : Yearly
To comply the legal requirement of quality control laboratory by calibration of lab.
balances & weight box by external agency.

5. 0 Reference Documents.:
1. Calibration of instruments file.
2. Bi monthly meeting MOM file.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

NATURAL GAS: (ADMINISTERED PRICE MECHANISM)

SR. NO. TEST SPECIFICATIONS.

1 METHANE 94.27
2 ETHANE 2.67
3 PROPANE 0.86
4 I-BUTANE 0.27
5 N-BUTANE -
6 I-PENTANE --
7 N-PENTANE --
8 HEXANE --
9 CARBON DIOXIDE --
10 OXYGEN 0.04
11 NITROGEN 1.89
12 NET CALORIFIC VALUE 8741 KCAL/NM3

NATURAL GAS: (RELIANCE INDIA LTD.)

SR. NO. TEST SPECIFICATIONS.

1 METHANE > 80% V
2 PROPANE AND HEAVY < 10 % V
3 OXYGEN < 0.2 %
4 CARBON DIOXIDE <3%
5 NITROGEN + OTHER INERT <5%
6 NET CALORIFIC VALUE ( MIN ) 7700 KCAL/SM3
7 SULPHUR < 10 PPM

AMMONIA:
SR.NO. TEST SPECIFICATIONS.
1 ANHYDROUS LIQUID AMMONIA 99.5% BY WT (MIN)
2 WATER 0.5% BY WT (MAX)
3 OIL 10 PPM (MAX)

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

CARBON DIOXIDE:

SR.NO. TEST BEFORE PASSIVATION AFTER PASSIVATION

1 CO2 97.88 % VOL (MIN) DRY BASIS 97.88 % VOL (MIN) DRY BASIS
2 INERT 1.25 % MAX. 1.0-2.0% MAX.
3 O2 NT 0.30-0.50%
5 H2 0.79 % MAX 1.5 % MAX

HDPE BAG:
SPECIFICATIONS
SR.NO. TEST STANDARD MIN. AVERAGE
VALUE VALUE VALUE
1 BAG WEIGHT 130 GM. 126.1 GM. 130 GM
2 WARP (KGF) 87 78.30 87
3 WEFT (KGF) 69 62.10 69
4 BOTTOM STRENGTH (KGF) 32 28.80 32

NOTE: MAXIMUM ALLOWABLE BAG HAVING MASS BETWEEN 126.1 GM TO 130 GM =

10 BAG MAX.

NEEM OIL:
SR.NO. TEST SPECIFICATIONS.
1 VISCOCITY AT 40 OC CST 40 - 55
2 DENSITY AT 25 OC 0.9100 – 0.9425
3 REFRACTIVE INDEX AT 40 OC 1.4632- 1.4700
4 CRACKING TEST NEGATIVE

FERTILIZER GRADE UREA:

SR.NO. TEST SPECIFICATIONS.

1 BIURATE 1.5 MAX.
2 MOISTURE 1.0 % MAX.
3 N2- 46.0 % MIN.
4 SIEVE
2.8 MM 10 % MAX.
2.8 MM TO 1.0 MM 80 % MIN.
< 1.0 MM 10 % MAX.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

NEEM COATED UREA:

SR.NO. TEST SPECIFICATIONS.
1 BIURATE 1.5 MAX.
2 MOISTURE 1.0 % MAX.
3 N2- 46.0 % MIN.
4 SIEVE
2.8 MM 10 % MAX.
2.8 MM TO 1.0 MM 80 % MIN.
< 1.0 MM 10 % MAX.
5 NEEM OIL 350 PPM MIN.

METHANOL:
SR.NO TESTS SPECIFICATION GRADE A/B/C

1 1) APPEARANCE CLEAR & FREE FROM SUSPENDED SOLIDS

2 METHANOL CONTENT (% WT.) MIN 99.9 / MIN 99.8 / BELOW 99.8

3 3) COLOR (APHA) < 15

4 4) WATER(PPM) 1000 MAX /2000 MAX / >2000

5 5) SP. GRAVITY AT 20 °C 0.792 – 0.798
6 6) ACIDITY INDEX 0.02 %WT MAX.
7 7) PERMANGANATE TEST 30 MINUTES, MIN.
8 8) NON – VOLATILE MATTER 0.001 % WT MAX.

ACETIC ACID:
TESTS SPECIFICATIONS GRADE A/B/C
SR.NO
CLEAR &FREE FROM SUSPENDED SOLIDS.
1) APPEARANCE
1
2 2) ACETIC ACID ( % WT ) MIN 99.8 /MIN 99.7 / BELOW 99.7%

3 3) FORMIC ACID (% WT ) 0.15 MAX / 0.15 MAX / ABOVE 0.15%

4 4) ACETALDEHYDE (% WT ) 0.03 MAX / 0.03 MAX / ABOVE 0.03%

5 5) WATER ( % ) 0.2 MAX / 0.3 MAX / ABOVE 0.3 %

6) COLOR (APHA)
15 MAX / 15 MAX / ABOVE 15
6
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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

MONO-METHYL AMINES

Sr.No. Test Specifications.

1 NH3 0.02 ( % WT MAX )
2 H2O 0.10 ( % WT MAX )
3 OTHER AMINES 0.30 ( % WT MAX )
4 MNO-METHYL AMINES 99.65 (% WT MIN.)

DI-METHYL AMINES

Sr.No. Test Specifications.

1 NH3 0.01 ( % WT MAX )
2 H2O 0.10 ( % WT MAX )
3 OTHER AMINES 0.20 ( % WT MAX )
4 DI-METHYL AMINES
99.70 (% WT MIN.)

TRI-METHYL AMINES

Sr. No. Test Specifications.

1 NH3 0.01 ( % WT MAX )
2 H2O 0.10 ( % WT MAX )
3 OTHER AMINES 0.20 ( % WT MAX )
4 TRI-METHYL AMINES 99.70 (% WT MIN.)

DIMETHYL FORMAMIDE

Sr. No. Test Specifications.

1 APPEARANCE CLEAR & FREE OF SUSPENDED SOLIDS
2 PH OF 20 % AQ 6.5 TO 9.0
3 COLOUR ( APHA ) <5
4 CH3OH ( PPM ) < 30
5 WATER ( % ) 0.08 MAX
6 CONDUCTIVITY OF 20% AQ 15 MAX
7 ACETIC ACID ( % WT ) NA
8 BASICITY AS DMA ( PPM ) 10 MAX
9 ACIDITY AS FORMIC ACID 5 MAX
(ppm)
10 PURITY (% WT MIN.) 99.85
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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 5 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

11 DENSITY GM/CC AT 20 DEG. C. 0.946 – 0.949

12 REFRACTIVE INDEX AT 25 1.4270 – 1.4285
DEG. C.

AMINES SOLUTIONS

PARTICULAR MMA DMA DMA TMA MMA

40% 40% 60% 30% 45%
MMA % WT 40.0 Min - - - 45.0 Min
DMA % WT 0.10 40.0 Min 60.0 Min - 0.1 Max
TMA % WT - 0.20 - 30.0 Min 0.02 Max
H2O % WT MAX 60.0 60.0 40.0 70 55.0

DIMETHYL ACETAMIDE

SR.
NO. TEST SPECIFICATIONS.
1 APPEARANCE CLEAR & FREE OF SUSPENDED
SOLIDS
2 PH ( RANGE ) 20 % AQUEOUS 4 TO 5
3 COLOUR ( APHA ) < 10
4 CH3OH ( PPM ) NA
5 WATER ( % ) 0.05 MAX
6 CONDUCTIVITY(RANGE) 20% < 40
AQUEOUS
7 ACETIC ACID ( % WT ) 0.1 MAX
8 PURITY (% WT MIN.) 99.75
9 DENSITY GM/CC AT 20 DEG. C. 0.935 – 0.942
10 REFRACTIVE INDEX AT 25 DEG. C. 1.4358 – 1.4360

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 6 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

FORMIC ACID :

Sr.No. Test FORMIC ACID

1 PURITY (% WT MIN.) > 85%
2 COLOUR (% WT MIN.) < 50 APHA
3 SULPHATE (% WT MIN.) MAX. 0.003%
4 CHLORIDE ( % WT MIN) MAX. 0.003%
5 NVM (% WT MAX.) MAX. 0.008%

AMMONIA SYNTHESIS GAS

SR.NO. TEST SPECIFICATIONS.

1 SYNTHESIS GAS ( CO + CO2 CONTENT) < 1 PPM
2 SYNTHESIS GAS ( MOISTURE CONTENT) < 5 PPM
3 PLANT INLET GAS ( DEUTERIUM) > 100 PPM

D.M. WATER :
SR.NO. TEST SPECIFICATIONS.
1 PH RANGE 6.5 TO 9.5
2 CONDUCTIVITY RANGE 1.0 TO 30 MICRO MHOS/CM.
3 SILICA < 0.02 PPM

HYDRAZINE HYDRATE:
SR.NO. TEST SPECIFICATIONS.
1 HYDRAZINE HYDRATE 80 % MIN
2 RELATIVE DENSITY AT 20 OC 1.05 GMS/CC
3 PH OF 1% SOLUTION 10.5 MIN

POTASSIUM CARBONATE:

SR.NO. TEST SPECIFICATIONS.

1 TOTAL ALKALINITY AS K2CO3 98 % MIN.
2 KOH 0.2 % MAX.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 7 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

3 CHLORIDE AS KCL 0.02 %

4 K2SO4 0.05 % MAX.
5 NA2O 0.08 % MAX
6 IRON 0.005 % MAX.
7 NICKEL 2 PPM

MORPHOLINE:
SR.NO. TEST SPECIFICATIONS.
1 PURITY % BY MASS 99 % MIN

TRI-SODIUM PHOSPHATE
SR.NO. TEST SPECIFICATIONS.
1 PHOSPHATE AS P2O5 BY MASS 17.5 % MIN

VANADIUM PENTOXIDE:
SR.NO. TEST SPECIFICATIONS.
1 APPEARANCE : RUST BROWN POWDER
2 VANADIUM CONTENT 99.5% AS V2O5
3 FORM : UN-FUSED GRANULAR POWDER 100 % PASSING THROU.30
MESH
4 SOLUBILITY LEVEL 100 % SOLUBLE IN 10 MIN. IN
30 % K2CO3 SOLN.
5 FE 0.05 % MAX.

DIETHANOL AMINE:
SR.NO. TEST SPECIFICATIONS.
1 APPEARANCE CLEAR LIQUID

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 8 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

2 COLOUR 25 APHA MAX.

3 SP.GR. AT 20 / 300 C 1.090 – 1.096
4 DEA CONTENT BY WT. 98 % MIN.
5 WATER CONTENT BY WT 0.3 % MAX.

SILICA GEL:
SR. NO. TEST SPECIFICATIONS.
1 PARTICLE SIZE 3 TO 6 MM
2 BULK DENSITY 0.8 - 0.9 GM/LIT
3 LOSS ON DRYING 6.0 % MAX.
4 ADSORPTION CAPACITY 25 % MIN
5 PH VALUE 3.5 – 8.0

ANION RESIN (NUCLEAR GRADE):

SR.NO. TEST SPECIFICATIONS.
1 EXCHANGE CAPACITY 0.8 MEQ/ML
2 MOISTURE CONTENT 60.0 % MAX.

CATION RESIN (NUCLEAR GRADE):

SR.NO. TEST SPECIFICATIONS.
1 EXCHANGE CAPACITY 1.8 MEQ/ML
2 MOISTURE CONTENT BETWEEN 50 TO 55 % MAX.

ANION RESIN FOR WATER TREATMENT:

SR.
NO. TEST SPECIFICATIONS.
1 IONIC FORM CHLORIDE
2 EFFECTIVE SIZE 0.5 – 0.6 MM
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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 9 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

3 EXCHANGE CAPACITY 1.20 MEQ/ML MIN.

4 MOISTURE CONTENT 50±2 %
5 SETTLED DENSITY 0.67 – 0.71 GMS/ML
6 PARTICLE SIZE < 50 U.S. MESH < 1.0 %
7 SCREEN SIZE 16 TO 50 U.S.MESH (WET)
8 WHOLE BEADS 95 %
9 CRACKS LESS THAN 5%

CATION RESIN FOR WATER TREATMENT:

SR.
NO. TEST SPECIFICATIONS.
1 IONIC FORM HYDROGEN
2 EFFECTIVE SIZE 0.5 – 0.6 MM
3 EXCHANGE CAPACITY 2.0 MEQ/ML MIN.
4 MOISTURE CONTENT 50±2 %
5 SETTLED DENSITY 0.80 – 0.84 GMS/ML
6 PARTICLE SIZE < 50 U.S. MESH < 1.0 %
7 SCREEN SIZE 16 TO 50 U.S.MESH (WET)
8 WHOLE BEADS 95 %
9 CRACKS HYDROGEN

SULPHURIC ACID:
SR.NO. TEST SPECIFICATIONS.
PURITY 98 % MIN.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 10 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

SODA ASH:
SR.NO. TEST SPECIFICATIONS.
1 TOTAL ALKALINITY AS A2CO3 % 98.5 % MIN

SODIUM CHLORIDE:
SR.NO. TEST SPECIFICATIONS.
1 PURITY 98 % MIN

SODIUM META-VANADATE:
SR.NO. TEST SPECIFICATIONS.
1 PURITY 82.5 % MIN

CAUSTIC SODA PURE:

SR.NO. TEST SPECIFICATIONS.
1 PURITY 95 – 99.5 %

POTASSIUM HYDROXIDE

SR.NO. TEST SPECIFICATIONS.

1 PURITY 98 % MIN.

GLYCINE

SR. NO. TEST SPECIFICATIONS.

1 PURITY 98 % MIN
2 LOSS ON DRYING < 0.5 %

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 11 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

COOLING WATER CHEMICALS: (M/S CHEMBOND)

SR. NO. PRODUCT TEST SPECIFICATION

PH ACIDIC
1 KEM WATREART 101 L+
SPECIFIC GRAVITY 1.28 MIN
PH ACIDIC
2 KEM WATREART 1002M +
SPECIFIC GRAVITY 1.04 MIN
PH ALKALINE, > 7.0
3 KEM WATREART BD
SPECIFIC GRAVITY 0.80 MIN
PH ALKALINE, > 7.0
4 KEM WATREART 3010 A
SPECIFIC GRAVITY 1.08 MIN
PH ALKALINE, > 7.0
5 KEM WATREART 304
SPECIFIC GRAVITY 0.8 MIN
PH ALKALINE
6 KEM WATREART 3020 M
SPECIFIC GRAVITY 1.10 MIN
PH ALKALINE
7 KEM WATREART BR +
SPECIFIC GRAVITY 1.14 MIN
PH ALKALINE
8 KEM WATREART CA 1
SPECIFIC GRAVITY 1.25 MIN
ZN ++ 10 % MIN.
9 KEM WATREART 101
PO43- 50 % MIN.
PH ALKALINE
10 KEM WATREART 305
SPECIFIC GRAVITY 0.85 MIN
PH 8.0 MIN
11 KEM WATREART 303
SPECIFIC GRAVITY 1.05 MIN.
PH ACIDIC
12 KEM WATREART 1002S SPECIFIC GRAVITY 1.17 ± 0.03
CALCIUM SEQ. VALUE 150 MG/ML (MIN.)
PH 12.5 ± 1.0
13 KEM WATREART B SPECIFIC GRAVITY 1.34 MIN.
ALKALINITY OF 10 % V/V 10 ML MIN.
PH 6.0 ± 1.5
14 KEM WATREART O
SPECIFIC GRAVITY 1.05 ± 0.03
PH ALKALINE
15 KEM WATREART 105 SPECIFIC GRAVITY 1.04 MIN
CALCIUM SEQ. VALUE 50 MG/ML (MIN.)
PH ALKALINE
16 KEM WATREART 3020
SPECIFIC GRAVITY 1.10

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 12 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

COOLING WATER CHEMICALS FROM VASU

SR NAME OF SPECIFIC
pH
NO. CHEMICAL GRAVITY
1 CORROSIL-908 ACIDIC 1.25 MIN
2 CORROSIL-144 ACIDIC 1.25 MIN

3 CORROSIL-S10 ZN++ : 10% PO4 : 50%

4 CORROSIL-213 ACIDIC 1.20 MIN

5 SCACIL-144 ACIDIC 1.04 MIN
CALCIUM
SEQ :
6 SCACIL-908 ACIDIC 1.08 MIN
150
mg/ml.
7 SCACIL-4144 ALKALINE 0.85 MIN
8 BIONIL-3908 ALKALINE 1.10 MIN
9 BIONIL-5144 ALKALINE 1.05 MIN
10 BIONIL-2144 ALKALINE 0.95 MIN
11 BIONIL-525BR ALKALINE 1.11 MIN
12 BIONIL-908C ALKALINE 1.20 MIN

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SPECIFICATIONS OF RAW MATERIAL AND PRODUCTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPEC-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 13 of 13
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

HEAVY WATER PLANT :

SR.NO. SAMPLE POINT SPECIFICATIONS.

1 12T1 GAS OUTLET ( DEUTERIUM) 20-25 PPM
2 CRACKED GAS OUTLET ( DEUTERIUM) > 0.9%
3 PURIFIER LIQ. ( AMIDE ) > 30 GMS.
4 12T1 LIQ. (AMIDE ) 20-25 GMS.
5 25V1( OLD) > 99.84%
6 18V10 A/B/C 30 – 40%
7 25V4 ( OLD) > 99.84%
8 12V2& 14C1 ( POTASSIUM CONTENT) < 1.0 PPM
9 REJECT FROM UGP ( NEW ) 150-500PPM

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: : TESTING OF RAW MATERIAL
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 20
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 10/05/2016

A) CENTRAL LAB

Analysis of natural gas and RIL gas

Analysis of natural gas is mainly guideline for optimizing plant process.
Analysis of natural gas is carried out using gas chromatographic technique on Chemito GC
with Thermal conductivity detector.
Chromatographic conditions
• Column: Porapack-Q
• Initial temp. 40OC (hold 2 min), Rate - 8OC/min.
• Final temp.- 180 OC ( hold 6 min )
• Injector - 50 OC
• Detector - 180 OC
• Carrier gas flow - 30 ml/min (Hydrogen)
Procedure for hydrocarbon analysis:
• Inject 1ml of sample in gas chromatograph; note the areas of the components.
• Calculate concentration of component using respective response factors.
• Result are recorded in TH-IMS/FR/QCL-CL/01-C is entered into SAP system. (Mat.
No. 570000067)
Analysis of Sulphur :
Reagents:
• 10 % Cadmium Acetate solution,
• Acetic acid.
• 0.025N Iodine,
• 0.025N Sodium thiosulphate
• Starch Indicator
Procedure:
• Take 50ml of 10% cadmium acetate and 50 ml acetic acid in the bubbler.
• Connect the bubbler assembly and gas flow meter to the sample point.
• Adjust the flow of the gas to 3 lit / min.
• Pass the gas through solution in the bubbler till the solution turns slightly yellow in
colour.
• Disconnect the assembly.
• To this solution add 25 ml freshly prepared 0.025 N iodine solution and titrate against
0.025N Sodium thiosulphate using starch indicator.
• End point is Blue to colourless.
• Take blank reading by titrating 50 ml of 10% cadmium acetate and 50 ml acetic acid
against sodium thiosulphate.

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: : TESTING OF RAW MATERIAL
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 20
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 10/05/2016

Calculations: (Blank – Sample) * N Na2S2O3 * 11.2 * 1000

Sulphur in ppm = ------------------------------------------------------
Total gas passed in liters

• Result are recorded in TH-IMS/FR/QCL-CL/01-E and entered into SAP system.

(Mat. No. 570000036)
LIQUID AMMONIA:
Analysis of liquid ammonia is done for oil and moisture.
• Reagents – Hexane
Procedure for Oil and moisture analysis:
• Collect carefully 1 lit of liquid ammonia in volumetric flask.
• Place the flask in fume hood.
• When complete ammonia is evaporated measure the volume of water remained.
• Calculate the moisture contained in Ammonia.
• Add 50 ml of AR grade hexane.
• Rinse the whole flask with hexane.
• Transfer the mixture to separating funnel.
• Transfer the hexane layer in platinum dish previously weighed.
• Rinse the flask twice with 50 ml of hexane.
• Evaporate the solvent on water bath and then place in oven for 30 min at 110OC.
• Finally place in desiccators until cool.

CALCULATIONS:
{ A x F x 0.890 x 0.684 x 100 }
% Moisture: = -------------------------------------------
V x 0.682

Weight of oil in gm x 106 x Eva. Factor.

Oil ppm = ------------------------------------------------------------
Vol. of sample in ml x Density of Ammonia (0.682)
Where

A : Volume of residue in ml

F : Evaporation factor

0.890 : Density of residue (gm/ml)

0.664 : Weight of fraction of water in residue

V : Volume of sample taken

0.682 : Density of sample
Result are entered into SAP system.( Mat. No. 570000044/570000045)

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: : TESTING OF RAW MATERIAL
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 20
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 10/05/2016

CARBON DIOXIDE
Analysis of carbon dioxide
Analysis of carbon dioxide is carried out using gas chromatographic technique on Fisher gas
partition chromatogram with thermal conductivity detector.
Chromatographic conditions
• Column: Porapack Q & Molecular sieve
• Oven temp. : 50OC
• Bridge current : 150 A
• Attenuator : 2
• Carrier gas flow - 30 ml/min (Argon)
Procedure for carbon dioxide analysis:
• Inject 1ml of sample in chromatograph; note the areas of the components.
• Calculate concentration of component using respective response factors.
• Result is entered into SAP system. (Mat. No. 570000109)

Neem oil analysis:

Neem Oil samples used for coating urea is tested for its Viscosity, Density, Specific gravity,
Crackling test, Appearance, and refractive index.
.
Appearance:
• Fresh oil appears clear and transparent. Due to contamination of water, ammonia and
some other chemicals it appears opaque.
Viscosity of oil sample:
• Viscosity is the property of the fluid whereby it tends to resists its relative motion within
itself. It should be measured at the required temperatures. It is measured with the help
of Brook Field viscometer in Centipoise.
Procedure:
• Switch “ON” the Brook Field viscometer.
• Connect the spindle No. 61.
• Dip the entire set up in oil to be tested up to marked level of spindle.
• Select RPM for maximum torque. Torque must be between 45 to 85.
• Selected RPM use for viscosity measurement.
• The reading will be displayed.
• Note the reading.
Convert centipoises to centistokes by
Centipoises / Sp.gravity = Centistokes
Specific gravity of oil sample:

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: : TESTING OF RAW MATERIAL
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 20
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APPROVED BY: HOD EFFECTIVE DATE: 10/05/2016

• The ratio of density of the substance at temperature under consideration to the density
of water at temperature of its maximum density, gives specific gravity of that
substance.
• Take oil sample in 250 ml measuring cylinder. Deep hygrometer of the range 0.8 to
0.9 in the oil and keep it floating. Mark the reading on the hygrometer up to which it is
dipped in the oil. This reading is a sp. gravity of the oil.

Acid No. or KOH value of oil:

• Oil is nothing but the higher fatty acids. KOH No. gives the acid No. of oil.
Reagents:
• Titration solvent
• Mixed indicator
• Alcoholic KOH
Procedure:
• Take 25 ml of oil sample and mix with approx. 50 to75 ml titration solvent. Add 2-3
drops of mixed indicator to it. Titrate this against 0.1 N KOH. Color change is from red
to green.
Calculation:
R * N KOH * 56.5
KOH No. = ---------------------------------------------
Sample volume * sp.gravity

Moisture content / crackling test:

• Oil and water are two immiscible liquids. Some chemicals also mixed with oil and
forms emulsion. Due to this oil appears milky.
Procedure:
• When such oil sprinkled on a heated hot plate, it gives crackling noise or foam which
indicates the presence of water with other chemical impurities.
• Water percentage should be measured by measuring cylinder.

Sampling procedure for polypropylene twine as per IS 12734 : 2002

1. Definitions:
a. Lot: The quantity of boxes / packages containing polypropylene twine of the
same construction supplied to one buyer against one dispatch note.
b. Package: Box / Package of spools.
2. Sampling procedure:
a. Draw the sample packages at random by using following formula,
S= 0.4 x N1/2
N= Total no. of packages in the lot; S = No. of packages to be selected
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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: : TESTING OF RAW MATERIAL
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 5 of 20
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APPROVED BY: HOD EFFECTIVE DATE: 10/05/2016

Sr. No of Select No. of

No. Packages packages( S )
received
1 01 to 13 1
2 14 to 37 2
3 38 to 74 3
4 75 to 120 4

b.From each package selected, draw at least five spools shall be drawn for tests.
Conformity tests

a. Breaking strength and Percent Elongation ( IS: 1670)

• Cut two specimens from a spool and check their strength and elongation.
• Average of these two specimen test results shall be considered as breaking
strength and percent elongation for that spool only.
• Check all the sample spools for strength and Elongation.
• Calculate average breaking strength and percent elongation of all the
sample spools.
• Consider this average for conformity of the lot.
• No tolerance limit provided for breaking strength.
b. Runnage ( m/kg )
• Check the runnage of spool having minimum and maximum breaking
strength.
• Remove 25 meter length and weigh. From the mass compute the length in
meter per kilogram.
• For conformity of the lot, test result of runnage satisfies the specified
requirement given in PO.

B) CHEMICAL GROUP LAB.

ANALYSIS OF METHANOL
1. Color and appearance
The sample shall be colorless and free from suspended material. Analysis of Color and
appearance is carried out using Spectrophotometer or Nessler’s tube.
Procedure:
• Read operating instructions from spectrophotometer manual.
• Load method file (i.e. meant for APHA) from the file menu of spectrophotometer.
• Use distilled water as blank and 10mm path length cell.
• Load the given sample to find out APHA value by using previously calibrated
spectrophotometer for APHA Method.
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• Record the result. ( APHA)

• Alternately the same can be measured by taking desired different APHA standards in
Nessler’s tube and match the sample color.
• Report the matched one standard as result ( APHA)

2. Moisture
Analysis of Moisture is carried out using Karl Fischer titrator.
Procedure:
• Take dried methanol in dry titration vessel of the previously calibrated Karl Fischer
titrator.
• Press “START” key.
• Weigh accurately the sample and transfer it to titration vessel.
• Enter weight of sample.
• Note the reading.
• Record your results.
3. Potassium permanganate Test
Potassium permanganate test is carried out using 0.01 N Potassium permanganate.
Procedure:
• Take 50 ml of sample in a Nessler’s tube.
• Add 1ml of 0.01 N potassium permanganate
• If pink color does not disappear within 30 minutes then test passes.
• If pink colors disappear within 30 minutes then test fails.

4. Specific Gravity
Specific Gravity determined using density meter.
Procedure:
• Switch “ON” the Density meter.
• Introduce the sample with the help of 2 ml plastic syringe.
• The reading will be displayed.
• Note the reading.
5. Non volatile matter (NVM)
Procedure:
• Take the weight of empty dry 100 ml evaporating dish as W1.
• To this add sample and weigh it as W2.
• Evaporate to dryness on water bath. Cool the evaporating dish in a desiccators.
• Take the weight of cool evaporating dish as W3.
• Calculate % NVM as follows.

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• Note the reading.

6. Acidity
Acidity is determined by consumption of 0.02N sodium hydroxide.
Procedure:
• Take known quantity of sample (50 ml approximately).
• Quickly added to titration vessel (conical flask or beaker) containing distilled water.
• Add two drops of phenolphthalein indicator.
• Titrate against 0.02N sodium hydroxide till pink color just appears.
• Calculate Acidity of sample as acetic acid.

• Note the reading.

ANALYSIS OF ACETIC ACID:

1. Color and appearance
The sample shall be colorless and free from suspended material. Analysis of Color and
appearance is carried out using Spectrophotometer or Nessler’s tube.
Procedure:
• Read operating instructions from spectrophotometer manual.
• Load method file (i.e. meant for APHA) from the file menu of spectrophotometer.
• Use distilled water as blank and 10mm path length cell.
• Load the given sample to find out APHA value by using previously calibrated
spectrophotometer for APHA Method.
• Record the result. ( APHA)
• Alternately the same can be measured by taking desired different APHA standards in
Nessler’s tube and match the sample color.
• Report the matched one standard as result ( APHA)
2. Purity
Assay of acetic acid by titration method.
Procedure:
• Take known quantity of sample.
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• Quickly added to titration vessel containing distilled water.

• Titrate against 0.5N sodium hydroxide.
• Note the burette reading.
• Calculate % assay as follows.

3. Formic acid:
Formic acid in acetic acid is done by iodometrc titration method.
Reagents
• Sodium hypobromide solution.
• 5% Potassium Iodide solution.
• 1:1 Hydrochloric acid
• Starch Indicator.
• 0.1N Sodium thiosulphate.
Procedure:
• Standardize the Sodium thiosulphate solution as per WI/
• Weigh accurately about 10 to 15 g of the sample in 500-ml clean iodine flask.
• Run reagent blank
• Slowly 20 ml of potassium iodide solution.
• 10 ml of 1:1 hydrochloric acid.
• Titrate against 0.1N sodium thiosulphate solution using starch as indicator.
• End point is blue to colorless
• Note the burette reading.
• Calculate % of formic acid as follows

4. Acetaldehyde
Acetaldehyde in acetic acid is done by iodometrc titration method.
Reagents:
• 1.25% Sodium Hydrogen Sulfite.
• 0.1N Iodine solution.
• Starch indicator.
Procedure:
• Weigh accurately about 10 to 15 g of the sample in 500-ml clean iodine flask.
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• Run reagent blank

• Add 50 ml of distilled water.
• Add 10 ml Sodium Hydrogen Sulfite solution.
• Stopper and Keep the flask in dark for 45 min.
• Titrate against 0.1N Iodine solution using starch as indicator.
• End point is colorless to blue.
• Note the burette reading.
• Calculate % of Acetaldehyde as follows

5. Moisture

Analysis of Moisture is carried out using Karl Fischer titrator.

Procedure:
• Take dried methanol in dry titration vessel of the previously calibrated Karl Fischer
titrator.
• Press “START” key.
• Weigh accurately the sample and transfer it to titration vessel.
• Enter weight of sample.
• Note the reading.
• Record your results.

Analysis of Carbon Monoxide Gas

Analysis of Carbon Monoxide is carried out using gas chromatographic
techni que on Mak- GC with Therm al conductivity detector.
Chromatographic conditions
• Column: Porapack –Q and Molecular Sieve
• Oven temperature: 70OC.
• Injector temperature: 100 OC
• Detector temperature: 150 OC
• Carrier gas flow - 30 ml/min (Argon )
• Elution order: Hydrogen, Argon-Oxygen, Nitrogen, methane and Carbon
monoxide.
Procedure for Carbon M onoxide analysis:
• Inject 1ml of sample in gas chromatograph on previously calibrated of desired gas
standard.
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• Match the retention time with the help of software.

• Calculate concentration of component using respective response factors.

C) HEAVY WATER LAB.

ANALYSIS OF SYNTHESIS GAS
CARBON MONOXIDE AND CARBON DI-OXIDE:
• Analysis of synthesis is carried out using gas chromatographic technique with flame
ionization detector
Chromatographic conditions:
• Column: Porapak Q/ Porapak QS: 1/8” x 8’ SS column packed with Porapak-Q or S.

• Oven temp.: 185OC.

• Methanator Temp. : 390OC
• Injector : 220OC ,
• Detector: 250OC.
• Carrier gas flow: 40ml/min ( Nitrogen)
• Hydrogen flow: 70ml/min,
• Inject 1ul of sample in chromatograph, note the areas of the components
• Compare sample area with the std area, find out the concentration of CO, CH4 &
CO2.
Moisture content:
• Analysis is carried out using dew point meter.
• Flush the instrument with sample gas for few minutes.
• Adjust the flow at 2 lit per min. Note down the dew point meter.
• Calculate the moisture.

Deuterium:
• Analysis is carried out using mass spectrometer.
• Inject few micro lts. of sample by glass ampoule.
• Standardize the instrument with two known lower ppm standards. ( in house
generated stds.)
• Range (20 to 120 ppm). Inject few micro liters of sample by glass ampoule.
• Record the D/H ratio with the help of computer.

D) WATER TREATMENT LAB.

Anion Resin:
Total exchange capacity:
• Exhaust 100 ml resin with sodium chloride.
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• Fill the resin in Column.

• Regenerate the resin by 1.0 N sodium hydroxide (Approximately 800 ml) with 15-20
ml/ min flow.
• Give DM water wash till the filtrate is neutral by adjusting same flow.
• Then give acid treatment to the resin with 25.0 % HCl (with 8 times of resin volume).
• Wash the column with DM water till the pH is 5.0.
• Take 35 ml of above resin in chloride form and pass 500 ml of 1.0 % sodium Nitrate
solution by adjusting same flow rate.
• Take 25.0 ml of filtrate in conical flask.
• Titrate it with 0.1 N silver nitrate solution using 5.0% potassium chromate indicator till
yellow to Reddish brown end point.
Calculation:
Reading × N of AgNO3 × 500
Total exchange capacity in chloride form ( meq / ml)= -------------------------------------------
35.0 × 25.0

Water retention capacity:

(Moisture holding capacity)
• Take around 10.0 - 20.0 gms of above resin by filtering through Whatman filter paper
no. 1.
• Weigh accurately in previously weighted crucible and dry it for 24 hrs in oven at
100ºC.
• After cooling in desicator weight it again and find weight loss and calculate moisture
holding capacity.
Calculations:
Weight loss × 100
% moisture holding capacity = ---------------------------
Initial weight of resin

Effective Size: Take 100 ml of resin in chloride form and sieve it through mesh no 16.0
A.S.T.M, 35.0 A.S.T.M, 45.0 A.S.T.M & 50.0 A.S.T.M and calculate effective size
Cation Resin:
.
Total exchange capacity:
• Exhaust 100 ml resin with sodium chloride.
• Fill the resin in Column and Regenerate by 1.0 N sodium hydroxide (around 400 ml )
with 15-20 ml/ min flow.
• Give DM water wash till the filtrate is neutral by adjusting same flow.
• Give acid treatment to the resin with 25.0% hydrochloric acid (with 4 times of resin
volume )
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• Then wash the column with DM water till the pH is 5.0.

• Take 35 ml of above resin chloride form and pass 500 ml of 5.0 % sodium chloride
solution by adjusting same flow rate .
• Take 50.0 ml of filtrate in conical flask.
• Titrate it with 0.1 N sodium hydroxide solution using phenolphthalein indicator till the
colour changes from colorless to pink

Calculation: Reading × N of AgNO3 × 500

Total exchange capacity in hydrogen form in meq / ml = -----------------------------------------
35.0 × 25.0

Water retention capacity:

(Moisture holding capacity)
• Take around 10.0 - 20.0 gms of above resin by filtering through Whatman filter paper
no. 1.
• Weigh accurately in previously decide crucible and dry it for 24 hrs in oven at 100ºC.
• After cooling in desicator weight it again and find weight loss and calculate moisture
holding capacity.

Calculations:
Weight loss × 100
% moisture holding capacity = ---------------------------
Initial weight of resin

Effective Size: Take 100 ml of resin in chloride form and sieve it through mesh no 16.0
A.S.T.M, 35.0 A.S.T.M, 45.0 A.S.T.M & 50.0 A.S.T.M and calculate effective size
SILICA GEL:
Procedure for Adsorption Capacity: -
• Fill the dried silica gel in previously weighted U glass tube and re-weight it, and find
the weight of silica gel
• Pass the ambient air through water to the one arm of the U tube.
• Allow the air to pass through the tube until no further increase in the mass of the tube
is observed..
Calculation: -
Increase in weight × 100
Adsorption Capacity in % = -----------------------------------------
Weight of silica gel

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ACTIVATED CARBON:
Iodine Value:
• Take accurately weighed about 0.2 gms of activated carbon (previously sieved
through 325 micron mesh) in a iodometrc 500 ml conical flask .
• Add 50.0 ml of 0.1 N Iodine Stopper the flask and keep it in a dark for 15.0 minutes.
Filter the content of conical flash through filter paper.
• Titrate with 0.1 N sodium thiosulphate solution using starch as an indicator. End point
is colorless to blue color.
• Run a blank reading also. Record the both reading.
Calculations:
(Blank - Sample reading) × N. of Sod. Thiosulphate ×126.91
Iodine Number in mg/ml = ------------------------------------------------------------------------------------
Weight of sample

COOLING WATER CHEMICALS:

Test to be carried out:
• pH
• Specific gravity
• Phosphate
• Zn
• Calcium sequestering Value
• Active Ingredient
Test Procedures:
pH: Ref. WRK/QCL/03.
Specific gravity: Ref. WRK/QCL/03.
Phosphate:
• Take 10.0 ml of 1.0 % solution of Kem Watreat chemicals in a 150 ml conical flask.
• .Add phenolphthalein indicator along with 1.0 gm of potassium oxalate.
• Titrate with 0.1 N Sodium hydroxide solutions.
• End point is colorless to pink color. Record the reading as T2.
• Then take another 10.0 ml of 1.0 % solution of Kem watreat chemical in 150 ml
conical flask & add 2-3 drops of bromocresol green indicator.
• Titrate it with 0.1 N sodium hydroxide solution.
• End point is yellow to green color. Record the reading as a T1.
Calculation: -
Phosphate in % = (T2 - T1) × 0.095 × 100
Zinc:
• Take 10.0 ml of 1.0 % solution of Kem Watreat chemicals in a 150 ml conical flash.
• Add 2.0 ml of pH-10 buffer solution and EBT Indicator.
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• Titrate this with 0.05 M EDTA solution and record the reading.
Calculation:
Zinc % = Reading × 65.38 × 0.05
Active Ingredient:
• Take 1.0 ml of Kem Watreat chemical in 250 ml beaker.
• Add 20 ml of 0.25 N potassium dichromate drop wise and shake it for 5.0 minutes.
• Filter the precipitate on whatman filter paper no.-41. Wash it with DM water, take the
filtrate & washing in a stoppered conical flask.
• To this add 50.0 ml of 6.0 % KI solution and 10.0 ml of HCl (6.0 N) immediately.
• Shake it well & allow it to stand in the dark for 5.0 minutes.
• Then titrate it with 0.1 N Na2S2O3 till end point of starch. Run a blank reading with
DW
Calculation:
% Active Ingredient = (Blank-Sample) × 2.45
Calcium Sequestering Value:
• Take 1.0 ml of Kem watreat chemical in 500 ml beaker.
• Add 50.0 ml demineralise water adjust the pH with NaOH to about 8.0. Add 10 ml of
2.0 % Na2CO3 solution. Adjust the pH to 9.0 with 1.0 N NaOH / acetic acid and bring
the total volume to 100.0 ml.
• Titrate this with 44.1 gms/lit calcium acetate monohydrate solution to a distinct and
permanent turbidity.
• Add the titrant solution in increment of 0.1 - 0.4 ml. .
• Stir well between each addition of calcium acetate solution. During titration, maintain
the pH to 9 by adding required amount of NaOH.
Calculation:
mgm/ml of Calcium sequestering value = Reading × 25.0
CHEMICALS:
Potassium Carbonate:
Purity:
• Take about 0.2 - 0.3 gm of dried material in a 250 ml conical flash.
• Dissolve it in 100 ml of DW and add 2-3 drops of Methyl Orange indicator.
• Titrate it with 0.2 N HCl. End point is yellow to red color.
Calculations:
Reading × 0.2 × 6.91
% Purity = -----------------------------------
Weight of material
Moisture :
• Take about 10.0 - 20.0 gms of material in previously weighted crucible.
• Dry it for 3.0 - 4.0 hrs in oven at 120.0 ºC.

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• Cool it in desicator and re weight it.

• Find the weight difference.
Calculation:
Weight difference × 100
% Moisture = -----------------------------------
Weight of sample.
Chloride:
• Take 1.0 gm of material in 100.0 ml Nessler’s tube add 10 ml DW .
• Neutralize with 1:1 HNO3 and 2 ml of 2.0 % AgNO3 Solution.
• Compared white turbidity produced with standard chloride turbidity on turbidity meter.
Iron:
• Take 1.0 gm of material in 100 ml Nessler tube add 10 ml of DW.
• Neutralize with 1:1 HCl and 5.0 ml of 10.0 % potassium thiocyanate solution.
• Compared red color produced with standard iron colors on spectrophotometer.
Sulphate:
• Take 1.0 gm of material in 100 ml Nessler tube.
• Add 10 ml of distillated water. Neutralize with 1:1 HCl and 5.0 ml of 10.0 % BaCl2
solution.
• Compared white turbidity produced with standard sulphate colors on turbidity meter.
Hydrazine Hydrate:
• Take about 2.5 - 3.0 gms of material in 500 ml volumetric flask, dilute to mark with DM
water. Then take 100 ml of DW in 500 ml iodometrc flask add 2.0 - 3.0 gm of NaHCO3
and 30.0 ml of 1:1 acetic acid. Shake well.
• Then add 5 ml above diluted sample to 50 ml of 0.1 n iodine solution.
• Prepare a blank along with the sample. Keep both the flask in dark for 30 minutes.
• Titrate this with Standard sodium thiosulphate solution using starch as an indicator.
Calculation: -
(Blank - sample)×N of Na2S2O3×100 × 0.0125 × 500
% Purity = ------------------------------------------------------------------------------
5.0 × weight in gms.
Sodium Bi sulphite: -
Purity:
• Take about 0.2 gm of material; add 50 ml of DW and 50 ml of standard iodine solution.
• Allow to stand for 5 minutes then add 1.0 ml of conc. HCl.
• Titrate the excess iodine with standard sodium thiosulphate solution using starch as
indicator. The end point reaction is indicated by disappearance of blue color.
• Carry out a blank titration with same amount of reagent but without sample.
Calculation:

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(B-S) × N of Na2S2O3 × 3.203

Purity (as SO2) % by mass = --------------------------------------
Weight of sample
Sulphuric Acid:
Purity:
• Take about 0.2 - 0.5 gms of acid in weighing bottle and put in to 500 ml beaker add 2 -
3 drops of methyl red indicator.
• Titrate this with 0.2 N NaOH solution till orange color persists.
Calculation:
Reading × N. of NaOH × 4.9
% Purity = ---------------------------------------
Weight of sample
TRI-SODIUM PHOSPHATE: -
Purity:
• Weight accurately 5.0 gms of material and dissolve it in beaker.
• Transfer in to 250 ml volumetric flask and make up to mark with demineralise water.
• Transfer above solution in to a conical flask and add 40-50 ml of barium chloride
(10%).
• All the phosphates and carbonates are precipitated off.
• Add 0.2 ml of phenolphthalein indicator and titrate with standard HCl solution to
colorless end point.
• Record this reading as a V1.
• Then take 25 ml of above solution in a conical flask .Add 0.2 ml of Methyl orange
indicator.
• Titrate against standard HCl solution to light pink end point.
• Record this as a V2 reading.
• To this flask add 35 - 40 ml of silver Nitrate solution ( 5.0 % ) and 2.0 ml of benzyl
alcohol to coagulate all the precipitate.
• Add 0.5 ml of M.O. indicator, and titrate the liberated nitric acid with standard NaOH
solution. The end point shall be from red to yellow, this will be V3 reading.
Calculation:
V3 × 3.55 × N of NaOH ×250
Phosphate (as P2O5) % by mass = ----------------------------------------
5.0 × weight of material
SODA ASH :
Purity:
• Take about 0.2 - 0.3 gms of dried material in a 250.0 ml conical flash.
• Add 100.0 ml DW and 2-3 drops of M.O.indicator and titrate it with 0.2 N HCl.
• End point will be yellow to red in color.
Calculations:
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Reading × N HCl. × 5.3

% Purity = -------------------------------
Weight of material
Moisture:
• Take about 10.0 - 20.0 gms of material in previously weighted crucible.
• Dry it for 3.0 - 4.0 hrs in oven at 120.0 ºC.
• Cool it in desicator and re weigh it.
• Find the weight difference.
Calculation:
Weight difference × 100
% Moisture = ---------------------------------
Weight of material
Chloride:
• Take 1.0 gms of material in 100.0 ml Nessler tube & add 10 ml DM.
• Neutralize with 1:1 HNO3 and 2.0 ml of 2.0 % AgNO3 Solution.
• White turbidity produced will be compare with chloride turbidity on turbidity meter
Iron:
• Take 1.0 gm of material in 100.0 ml Nessler tube add 10 ml DW.
• Neutralize with 1:1 HCl and 5.0 ml of 10.0 % potassium thiocyanate solution.
• Red color produced is to be comparing with standard iron colors on
spectrophotometer.
Sulphate:
• Take 1.0 gms of material in 100.0 ml Nessler tube add 10 ml DW .
• Neutralize with 1:1 HCl and 5.0 ml of 10.0 % BaCl2 solution.
• White turbidity produced will be compared with standard sulphate colors on turbidity
meter.
DI ETHANOL AMINE :
Purity:
• Take about 0.2 - 0.5 gms of material in 250 ml dried conical flask and add 50 ml of
DW.
• Add 2 - 3 drops of methyl red indicator and titrate it against standard HCl solution.
• Record the reading and calculate the % purity of material.
Calculation :
Reading × N of HCl × 10.54
% purity = ------------------------------------
Weight of material
SODIUM CHLORIDE:
Purity:
• Take about 0.2 - 0.4 gms of material in a dried conical flask add 100 ml DW.

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• Add 2-3 ml (5.0 %) potassium chromate indicator and titrate against silver nitrate.
• End point shall be yellow to radish brown.
Calculation:
Reading × N of silver nitrate × 0.0585 × 100
% purity = --------------------------------------------------------
Weight of the material
BLEACHING POWDER: -
Purity:
• Take about 0.2 gms of material in a dried iodometric conical flash.
• Add 0.5 gms of potassium iodide and 20 ml 1:1 HCl.
• Keep this in dark for 10 minutes.
• Then titrate with 0.1 N potassium thiosulphate solution using starch as an indicator
Calculation:
Reading × 0.1 × 0.03555 ×100
% of Chloride = -------------------------------------
Weight of material
MORPHOLINE: -
Purity:
• Take about 0.4 - 0.6 gms of the material in a dried 250 ml conical flask add 1-2 drops
of methyl orange indicator
• Titrate against standard hydrochloric acid till colour changes from yellow to orange.
Calculation:
Reading × 8.712 × N of HCl
% Purity = -----------------------------------
Weight of material
ETHYLENE GLYCOL: -
• pH: Ref. WRK/QCL/03.
• Specific gravity: Ref. WRK/QCL/03.

SODIUM META VANADATE:

Purity:
• Dissolve 0.2 gms of material in 25 ml H2SO4 add 200 ml DW and 5 ml phosphoric
acid.
• Cool with ice add 10 ml of 0.1 N ferrous ammonium sulphate solution and stir for 10
minutes. Add 8 ml of freshly prepared (15.0 %) Ammonium persulphate solution.
• Stir for 1 minute and then titrate it with 0.1 N potassium permanganate solution till pink
color persist for 1 minute.
Calculation: -
% NaVO3 = Reading × 12.3

18
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TITLE: : TESTING OF RAW MATERIAL
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POTASSIUM ANTIMONY TARTARATE:-

Purity:
• Dissolve 0.8 gms of the material in 50 ml DW.
• Add 8 gms of potassium sodium tartarate and 1 gm of sodium hydrogen carbonate
and titrate against 0.1 N iodine solution.
• Iodine acts as a self indicator.
Calculation:
1 ml of 0.1 N iodine ≅ 0.01625 gms Potassium antimony tartarate / Weight of material
TARTARIC ACID:
Purity:
• Dissolve 3.0 gms of the dried material in 100 ml DW.
• Titrate against standard sodium hydroxide solution using phenolphthalein indicator.
Calculation: -
Reading × N of sodium hydroxide × 7.505
% Purity = --------------------------------------------------------
Weight of material

VANADIUM PENTOXIDE: -
Purity:
• Take 0.51 gms of the material.
• Add 70 ml nitrosulphuric acid solution ( 2 : 1 : 2 HNO3: H2SO4:H2O).
• Digest on hot plate for 90 minutes.
• Cool at RT and dilute with 200 - 300 ml distillated water.
• Again heat to boil and cool to R.T. (15.0 °C).
• Add potassium permanganate to deoxidize.
• Add 70 ml 0.1 N ferrous ammonium sulphate & add 30 ml of (20 %) Ammonium
persulphate.
• Check the above solution for spot test with K3 Fe(CN)6 .
• And then titrate against 0.1 N potassium permanganate solution.
Calculation:
Reading × 0.1 × 0.5095 × 1.785
V2O5 % = ------------------------------------------------
Weight of material
CAUSTIC SODA LYE:
Purity:
• Take about 0.3 - 0.4 gms of the sample in weighing bottle
• Add in to the 500 ml beaker containing 200 ml DW.
• Then add 2 - 3 drops of methyl red indicator.

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• Titrate against 0.2 N NaOH solution.

• At end point colour changes from.yellow to orange
Calculation:
Reading × N of NaOH × 4.0
% Purity = ------------------------------------------
Weight of material

QUICK AND HYRDATED LIME:

Purity:
• Dissolve accurately weighted 2.5 gms of material in a minimum quantity of
concentrated HCl and make up to 1000 ml with distilled water.
• Pipette out 10 ml of above solution in 250 conical flasks and dilute with 40ml DW.
• Add 1.5 ml of 1.0 N NaOH solution and 0.1 - 0.2 gms of Muroxide indicator
(or 0.07 gms of calcon indicator).
• Titrate against standard E.D.T.A. solution till color changes from wine red to purple.
( For calcon indicator the color change will be from greenish to yellow fluorescence to
brown)
• Note the burette reading.
Calculation:
Reading × N of E.D.T.A. × 14.02 × 1000
Total calcium oxide (as CaO) % by mass = --------------------------------------------------------
wt of sample in gms. × 10
POTASSIUM HYDROXIDE:
Purity:
• Take about 0.3 - 0.5 gms of material and add into 200 ml distilled water.
• Add 2 - 3 drops of methyl orange indicator.
• Then titrate it against 0.2 N HCl till colour changes from yellow to orange.
• Record the titrate value.
Calculation: -
% Purity = (Reading × N of HCl × 5.6) / Weight of sample

20
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

A) CENTRAL LAB.

Sulfur content in ZnO Absorber outlet:

Reagents:
• 10 % Cadmium Acetate • 0.025N Sodium
solution, thiosulphate
• Acetic acid. • Starch Indicator
• 0.025N Iodine,
Procedure:
• Take 50 ml of 10% cadmium acetate and 50 ml acetic acid in the bubbler.
• Connect the bubbler assembly and gas flow meter to the sample point.
• Adjust the flow of the gas to 3 lit / min.
• Pass the gas through solution in the bubbler till the solution turns slightly
yellow in colour.
• Disconnect the assembly.
• To this solution add 25 ml freshly prepared 0.025 N iodine solution and
titrate against 0.025N Sodium thiosulphate using starch indicator.
• End point is Blue to colourless.
• Take blank reading by titrating 50 ml of 10% cadmium acetate and 50 ml
acetic acid against sodium thiosulphate.
Calculations:
(Blank – Sample) * N of Na2S2O3 * 11.2 * 1000
Sulphur in ppm = ------------------------------------------------------
Total gas passed in liters
• Result are recorded in TH-IMS/FR/QCL-CL/01-E and entered into SAP system.
(Mat. No. 570000036)

GAS ANALYSIS:
Process gas samples:
• PRO, HTI, HTO, MTO, LTO, ABS, METH, S-300-IN, S-50-IN, S-50-
OUT,TO HWP, FROM HWP .
HGRU samples:
• Hydrogen PRODUCT, MEM-IN, MEM-OUT(TO-ARGON), PURGE, FROM
Argon
• (P1,P2,P3,P4,P5,P6,P7,P8)BEDS, (S1,S2,S3,S4,S5,S6,S7,S8) BEDS,
PRI-OUT
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Chromatographic condition:
• Column : Porapack Q & Molecular sieve
• Carrier gas flow (H2) :30 • Detector temp : 150 0C
ml/min • Detector type :TCD
• Injector temp.:500C • Bridge current :175 mA
• Oven temp : 800C
• Elution pattern :CO2 , O2 ,N2 ,CO and CH4
• Record the results in process gas register & enter into SAP system.
(Mat.No.10000012 for Ammonia line I and 10000013 for Ammonia line II)

Ammonia from gas samples:

• Sample is purged through glass bomb. Gas containing ammonia is trapped in
bomb by closing two side valves. Pressure is released by opening one side
valve and then water is added. Ammonia from gas is dissolved in water.
Ammonical water is titrated against 0.2 N HCL by using mixed indicator.
Rd X Normality X 22.4 X 100
• % Ammonia = ------------------------------------
Volume of sample in ml* 0.85
• Note.: While purging connect rubber tube at the other end of glass bomb to
dissolve ammonia in water.

Urea prills:
1) Sieve analysis:
• Weigh 100 gm of sample and pass the sample through sieves as given below.
• Weigh the sample retain on each sieve and also in the last tray.
• +2.8 mm , -2.8 + 2.4 mm, -2.4 mm + 1.7 mm, -1.7 mm + 1.0 mm, -1mm

2) DETERMINATION OF BIURET CONTENT IN NEEM COATED UREA

Reagents :
Alkaline tartarate solution --- Dissolve 40gms of NaOH in 50ml of water cool add 50
gms of NaKC2H4O and dilute to 1 litre. Let it stand for one day before use.
Copper sulphate solution --- Dissolve 15 gms of CuSO4.5H2O in CO2 free water
and dilute to 1litre.
Biuret standard solution ---- 2mg/ml. Dissolve 200 mgms of reagent grade biuret in
CO2 free water and dilute to 100 ml.
Preparation of standard curve :
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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With a burette transfer series of aliquots. 2 -5 – 15 – 25 – 40 -50 ml of a biuret

standard solution corresponding to 4 – 10 – 30 – 50 – 80 – 100 mg of biuret solution
in 100 ml volumetric flask.
Adjust vol. to approximate 50ml with Co2 free water. Add one drop of methyl red
indicator and neutralize with 0.1n H2SO4 to pink colour.
Add with swirling 20ml of alkaline tartarate solution and then 20ml of CuSO4
solution.
Dilute to the volume --- shake for 10 seconds and place in water bath for 15 minutes
at 30±5 ᴼC.
Also prepare reagent blank.
Determine absorbance of each solution against blank at 555 nm with 10 cm cell, and
plot standard curve.
Procedure for biuret % in Urea:
Stir continuously 25 gms of sample in 100 ml approximately 50ᴼC water for 30
minutes.
Filter and wash into 250 ml of volumetric flask and dilute to volume.
Transfer 25ml aliquot tom 100ml volumetric flask and proceed as given under
preparation of standard curve.
Calculation:
From standard curve determine concentration of biuret in final dilution. Then
C × 100
% Biuret = --------------
W
Where C = concentration in mg/ml of biuret in final dilution obtained from
standard curve.
W = comcentration of original sample in final dilution expressed.
( Reference ----- Methods of Analysis, AOAC. 1965 )
3) Moisture:
Refer Karl Fisher method for Moisture determination of Methanol.( WRK/QCL/01)

4) Total Nitrogen:
Reagent: -
• Concentrated H2SO4 • 0.2 N NaOH.
• K2SO4. • 0.2 N H2SO4
• Selenium powder • Methyl Red Indicator.
• 40% Caustic
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Procedure:
• Take 0.2 gm sample in Foss tube.
• Add 15 ml of Conc. H2SO4 and 7 gms of K2SO4 with pinch of Se Powder.
• Digest for 40 minutes on Foss digester at 410oC until white fumes stops.
• Cool the all tubes for 15 minute.
• Fix the tube on Foss distillation unit.
• Take 50 ml of 0.2N H2SO4 in the conical flask and dipped tip inside acid.
• Run the program 1(80 ml distilled water + 50 ml alkali + steam distillation )
• Titrate the distillate with 0.2 N NaOH using methyl red indicators.
• End point is red to yellow
• Run reagent blank by titrating 50 ml of 0.2N H2SO4 with 0.2N NaOH.
Calculation:-
(Blank – Reading) X N of NaOH X 1.4008
% Total N2 = -----------------------------------------------------------
W e i g ht o f sa mp l e

5) Determination of Oil in Neem coated Urea.

Regents:
• Hexane AR/GR grade. • Dilute HCl.
Procedure:
• Weight accurately about 200 gm Neem coated urea and transfer it to a 1000 ml
separating funnel. Add about 250 to 300 ml warm distilled water and shake
gently to dissolve urea acidify with 5 ml. dil. HCl.
• Extract the oil using 50 ml hexane and separate the oily hexane layer.
• Repeat the extraction of oil from the aqueous layer with 50 ml fresh hexane.
• Give washing to this oily hexane with warm distilled water till it is completely free
from urea. Transfer the hexane layer to an oil free 100 ml beaker. Give the 2-3
washings to the separating funnel with about with about 10 ml hexane each time
to transfer completely the oil from the separating funnel to the beaker.
• Heat the contents in the beaker on a water bath to break any emulsion formed.
Filter this oily layer into another previously weighed 100 ml beaker.
• Give to two to three (10 ml) hexane washings to the filter paper to transfer the oil
completely into the weighed beaker.
• Evaporate hexane by keeping beaker on water bath at 105 0C for about two
hours. Cool in desiccators and weigh the contents to a constant weight. Find out
the weight of this oil in the beaker.
• Carry out a blank test with hexane (with equivalent amount consumed in the test)
for oily content present, if any and subtract the same from the test results.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Calculation:
• Weight of urea sample = W gm
• Weight of oily layer = X gm
• Weight of oily layer for blank = Y gm
(X-Y) x 106
Neem oil in ppm = -----------------
W
REACTOR, STRIPPER, ME2, ME3, V3, MV52 SAMPLES (Mat No. 570000119)

• Take approx. 100 ml of distilled water in conical flask and weigh it. In this
Collect about 40 to 80 gm of sample from Reactor, Stripper, ME2 (i.e.
M.P. decomposer), ME3 (i.e. L.P. decomposer), V3, MV52 respectively.
• Cool for some time and again weigh the conical flask.
• Now transfer the sample to 1000ml volumetric flask and make up with
distilled water.
The following tests are conducted using this sample.

1) TOTAL AMMONIA %: (for effluent samples also).

Reagents:
• 0 .2N HCl
• Mixed indicator
Procedure:
• Take 10ml sample in conical flask.
• Add 2-3 drops of mixed indicator.
• Titrate against 0.2N HCl.
• End point is Green to pink color.

Calculations:
R x NHCl x 0.017 x 100 x 1000
% Total NH3 = -----------------------------------------
Wt. of sample x 10
2) % UREA:
• Take 10 ml sample in porcelain dish.
• Weigh the porcelain dish (Initial weight).
• Evaporate on water bath till dryness.
• Cool in desicator and weigh again. ( final weight )
Calculation:
( Final Wt – Initial weight )X 1000X100
% of Urea = ------------------------------------------------
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Wt. of sample X 10
3) % FREE NH3:
Reagents:
• 12 % BaCl2 • Mixed Indicator
• 0.2 N HCl
Procedure:
• Take 50 ml sample in 500 flask.
• Add 150 ml of BaCl2 solution and dilute with 500 ml DW. water.
• Keep in dark for 2 Hrs.
• Take 10 ml diluted sample in conical flask.
• Add mixed indicator & titrate against 0.2 N HCl.
• End point is green to pink.
Calculation:
R x NHCl x 0.017 x 100 x 1000
% Free NH3 = -----------------------------------------
Wt. of sample x 50

4) % CO2:
% CO2 = ( % T.NH3 - % Free NH3 % ) * 1.292
5) % H2O:
% H2O = 100 – ( % T. NH3 + % CO2 + % UREA)

GV solution analysis:

1) K2CO3 & KHCO3

Reagents:
• 1 N H2SO4
• Phenolphthalein indicator
• Methyl Orange indicator

Procedure:
Weigh about 2 ml of solution and transfer them quantitatively into a 400-ml
beaker. Dilute the sample with 50-80 ml of demineralised water and titrate with H2SO4
1N . Record the readingup to its completion.

Expression of results
% K2CO3 = ( 13.82 X A)/ W
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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% KHCO3 = 10.01 X(B- 2A)/W

% KHCO3 (as % K2CO3) = % KHCO3 × 0.691
% Equivalent K2CO3 = % K2CO3 + % KHCO3 (as % K2CO3)
(
FC =% KHCO3 as% K2CO3 )/% Eq.K2CO3
where:
A = ml of H2SO4 1N used ( First end point )
B = ml of H2SO4 1N used (second end point)
w = weight in grams of solution withdrawn for analysis.

2) Density : Take weight of 10 ml sample. Note down the density as Gms/cc.

Record in shift log book. & enter in sap.

3) Iron:
Reagents:
• HCL 1:1
• KSCN 10 %
• Std. Iron solution ( 1ml = 0.1mg of iron)
Procedure:
• Take 50ml sample in Nessler’s tube.
• Add 2ml 1:1 HCL and 5ml 10 % KSCN. Also prepare blank.
• Allow the color to develop for about 10 to 15 min. Measure the concentration on
spectrophotometer at wavelength 410nm

4) DEA (Diethanol Amine)

Reagents:
• 1 2 .5 N H3PO4 • Solid CuCO3
• 10.5 N KOH
• Std. GV soln. ( 36 gms K2CO3 + 1.2 gms Glycin + 0.5 gmsV2O5 ) dilute
to 100 ml volumetric flask with DM water.
Procedure:
• Take 5 gms of GV solution in 100 ml volumetric flask.
• Add 10 ml of 12.5 N H3PO4, heat to boil off CO2 and cool.
• Add 20 ml of 10.5 N KOH. Bring the volume to the mark in 100 ml flask
with DM water.
• Add 1gm of CuCO3 shake continuously for 20 minutes.
• Filter out through sintered crucible G3 under vacuum and collect filtrate in
standard tube.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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• Run blank with 5 gms of standard GV solution along with same addition of
above reagents.
• Measure absorbance at λ. = 650 nm on DEA-GV file.
Calculation:-
• % DEA = A x K / W x 10
• A= absorbance of sample
• K= Factor ( 184.664 according to DEA-GV file)
• W= Weight of sample.

5) Vanadium Analysis:
Reagent:
• 30 % K2CO3 • 2 % Hydroxylamine hydrochloride
• Pure glacial acetic acid. solution
Procedure:
• Take three 100 ml volumetric flasks (A-B-C)
• Weigh 20 grams of GV solution and transfer it in flasks B & C.
• Take 25 ml 30 % K2CO3 solution in flask A i.e. blank.
• Then according to equivalent K2CO3, add 30% K2CO3 solution in flask B& C
from table.
• Add 25 ml acetic acid in all flasks with constant stirring with due care.
• Add 5 ml of 2% Hydroxylamine hydrochloride solution in flask A & C.
• Boil all flasks for 2 to 3 minutes to expel out CO2.
• Cool the flasks to room temperature and make up to the mark.
• Measure concentration on spectrophotometer on file N-V2O5.

Calculation:
• Total vanadium % as V2O5=A/W*10
• A = mg of V2O5.
• W = wt. of sample.
• % V+4 as V2O5 = % V2O5 in flask B.
• %V+5 as V2O5 = (% V2O5 in flask C) – (% V2O5 in flask B)
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Reference table for 30% K2CO3:-

% Eq. K2CO3 30% K2CO3 to be added

20 14.6 ml.
22 13.6
24 12.5
26 11.6
28 10.6
30 9.3
Preparation of Curve of standard V2O5 solution:
• Weigh 2 grams of V2O5, dissolve in 30% K2CO3 and make up to 100 ml with 30
% K2CO3. it will give 1ml = 20 mg of V2O5 .
• Take 0, 2, 4, 6,8,10, 12 ml of standard solution in 100 ml volumetric flask.
• Add K2CO3 solution to each flask to obtain total volume 25 ml.
• Slowly add 25 ml acetic acid + add 5 ml hydroxylamine hydrochloride and boil for
2 minutes then cool and make up to 100 ml. with distill water.
• Plot a calibration curve at wavelength 785 mm.

6) GLYCINE ANALYSIS IN GV SOLUTION.

Reagent:
• Concentrated H2SO4 • 0.2 N NaOH.
• K2SO4. • 0.2 N H2SO4
• Selenium powder • Methyl Red Indicator.
• 40% Caustic
Procedure:
• Take 20 gms of GV Solution in Foss tube.
• Add 15 ml of Conc. H2SO4 and 7 gms of K2SO4 with pinch of Se Powder.
• Digest for 40 minutes on Foss digester at 410oC until white fumes stops.
• Cool the all tubes for 15 minute.
• Fix the tube on Foss distillation unit.
• Take 50 ml of 0.2N H2SO4 in the conical flask and dipped tip inside acid solution.
• Run the program 1 ( 80 ml distilled water + 150 ml alkali + steam distillation )
• Titrate the distillate with 0.2 N NaOH using methyl red indicators.
• End point is red to yellow
• Run reagent blank by titrating 50 ml of 0.2N H2SO4 with 0.2N NaOH.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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• Calculation:-
(Blank – Reading) X nom. of NaOH X 1.4008
% Total N2 = -----------------------------------------------------------
Weight of sample
Calculation:
% Glycine = (TN- DEAN) x 75.01/14
= (TN- DEAN) x 5.358
7.0) Foam Test:
• Take 50 ml sample in 250 ml graduated cylinder ( at 80-90 0C)
• Connect inert gas nitrogen to the one end of the Sparger tube through rota meter.
Sparger is rest on the bottom of the cylinder and maintain the flow the gas i.e. (40-50
liter / hrs)
• Record the highest foam peak in mm (within 3 minutes from the start of the N2 flow.
(Foaming is excessive if the foam peak is highest than 40 mm during N2 bubbling.)
• Cut the N2 flow and record the collapse time i.e. when the foam is broken and
disappears in the centre of the superficial liquid layer. (Foaming is excessive if collapse
time is more than 15 seconds.)
• Result of three tests have to be compared

BAG TESTING (Mat. No. 250000005)

As per NIT MX-20363 dated Jan’2015, three Lots of HDPE Sample Bags receives in
the laboratory for destructive testing. Sample lot size drawn is as per IS : 9755 – 2003.
Sample Bags received are first checked for sign, identification mark and number
written on bags as per forwarding. Select 40 % bags ( IS- 9755:1999 ) and give them number
as per pattern, fold them and keep aside. These bags are used for mass as well as
destructive testing. Fold remaining bags. Take mass of all these folded bags of the lot.

For destructive testing, use these 40 % bags. Mark and cut the specimens of 5 by 20
cm. (Reveled strip test, IS 1969 : 1985) for widthwise & lengthwise portion of the bag and
also cut the specimen for Bottom Seam as per cut strip test IS 9030 : 1979. Check the
strength and % elongation on computerized Tensile Testing Machine with constant traverse
speed of 300 mm/min.

Accordingly report is generated to get pass/fail status of the lot.

Now as per NIT MX 20363 ( 2015 ), if lot I fails in one or more parameters, Lot II is tested in
our lab. Lot II is tested only for the fail parameters of lot I. If Lot II is failed in one or more
parameters, Lot III will be tested in Trombay lab / Thal lab in presence of supplier'
representative / III party. Lot III is tested for the fail parameters of Lot I.
Then that lot is declared as pass or fail.
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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Dew point: Refer TH-IMS-QCL-WRK-01

Vessel Entry permit air Sample:

• During plant Shut down, Air sample from various vessels are collected for entry permit.
• These samples are collected in bladders by suction / vacuum pump.
• They are tested for hazardous gas like NH3, CO, CO2 and for oxygen content.
• Testing as per WRK/QCL/03.
Flue and vent gas Sample:
• Plant vents samples and Flue gas from Furnace and Boilers are collected in
bladders by suction / vacuum pump.
• They are tested for hazardous gas like NH3, CO, CO2 and for mainly for oxygen
content.
• Testing as per WRK/QCL/03.

Oil Sample:
Oil samples of rotating equipment from plant are tested for its Viscosity, Specific
gravity, Acid No. KOH Value, Colour , Appearance and moisture content.
Refer QCL/WRK/01 (Neem oil analysis)
Moisture content / crackling test:
• Oil and water are two immiscible liquids. Some chemicals also mixed with oil and forms
emulsion. Due to this oil appears milky.
Procedure:
• When such oil sprinkled on a heated hot plate, it gives crackling noise or foam which
indicates the presence of water with other chemical impurities.
• Water percentage should be measured by measuring cylinder.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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B) CHEMICAL GROUP LABORATORY

ANHYDROUS AMINES: SPECIFICATIONS

PARTICULAR MMA DMA TMA

NH3 % WT Max 0.02 0.01 0.01
H2O % WT Max 0.10 0.1 0.1
OTHER AMINES % WT Max 0.30 0.20 0.20
PRODUCT PURITY % WT Min 99.65 99.70 99.70

Anhydrous amines from old and new plants are analyzed on gas chromatograph having
thermal conductivity detector. Typical gas chromatograph conditions are

Chromatographic conditions
• Column: Porapack–Q coated with 10% TEPA and 1 M potassium hydroxide.
• Oven temperature: 90OC. • Current: 150 mA
O
• Injector temperature: 150 C • Carrier gas flow: 30ml/min (H2)
• Detector temperature: 150OC
• Elution order is Ammonia,MMA,DMA,TMA,CH 3 OH,H 2 O
Procedure:
• Inject 1ml anhydrous (vapor) sam ple in GC on previously calibrated with desired
standard.
• Match the retention time with the help of software.
• Calculate concentration of com ponent using respective RF.
 DEPARTMENTAL IMS MANUAL
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AMINES SOLU TION AQUEOUS: SPECIFIC ATIONS

PARTICULAR MMA DMA DMA TMA MMA

40% 40% 60% 30% 45%
MMA % WT 40.0 Min - - - 45.0 Min
DMA % WT 0.10 40.0 Min 60.0 Min - 0.1 Max
TMA % WT - 0.20 - 30.0 Min 0.02 Max
H2O % WT MAX 60.0 60.0 40.0 70 55.0

Amine solutions

Amines solutions from old and new plants are analyzed by consumption of acid.

Procedure for amines solutions

• Weigh accurately about 0.2 to 0.4 g of the sample.
• Add about 20ml distilled water and a drop of bromothymol blue indicator.
• Titrate against 0.2 N Hydrochloric acid solutions.
• End point is blue to yellow.
• Note the burette reading.
• Calculate concentration of amine as follows,
% amine = Burette reading x N HCl x F / wt. of sample
• For analysis of MMA, DMA and TMA use following factors respectively ,

Sr.No. Amines F
1 MMA Solution 0.031
2 DMA Solution 0.045
3 TMA Solution 0.059
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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DIMETHYL FORMAMIDE:
Analysis of N,N Dimethyl formamide (DMF) samples in process and finished products is
carried out regularly to ensure specified quality of the product. The samples are tested for
different parameters as follows,

Sr.
No. Test Specifications.
1 APPEARANCE CLEAR & FREE OF SUSPENDED SOLIDS
2 COLOUR ( APHA ) <5
3 pH 6.5 TO 9.0
4 CONDUCTIVITY 15 MAX
5 DENSITY GM/CC AT 20 DEG. C. 0.946 – 0.949
6 REFRACTIVE INDEX AT 25 DEG. C. 1.4270 – 1.4285
7 WATER ( % ) 0.08 MAX
8 ACIDITY AS FORMIC ACID ( PPM ) 5 MAX
9 BASICITY AS DMA ( PPM ) 10 MAX
10 CH3OH ( PPM ) < 30
11 DMAC IMPURITY IN DMF < 100 PPM
12 PURITY (% WT MIN.) 99.85

1. Color and appearance

The sample shall be colorless and free from suspended material. Analysis of Color and
appearance is carried out using Spectrophotometer or Nessler’s tube.
Procedure:
• Read operating instructions from spectrophotometer manual.
• Load method file (i.e. meant for APHA) from the file menu of spectrophotometer.
• Use distilled water as blank and 10mm path length cell.
• Load the given sample to find out APHA value by using previously calibrated
spectrophotometer for APHA Method. Record the result as APHA
• Alternately the same can be measured by taking desired different APHA standards in
Nessler’s tube and match the sample color.
• Report the matched one standard as result ( APHA)
2. 0 pH of 20% aqueous DMF solution:
pH is carried out using previously calibrated pH Meter.
Procedure:
• Take 20ml of DMF.
• Add 80ml of distilled water & stir.
• Measure the pH
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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3.0 Conductivity of 20% DMF solution:

Conductivity is carried out using previously calibrated Conductivity Meter.
Procedure:
• Take 20 ml of DMF.
• Add 80ml of distilled water & Stir.
• Measure the conductivity.
4.0 DENSITY at 20O C
Density determined using previously calibrated density meter.
Procedure:
• Switch “ON” the Density meter.
• Introduce the sample with the help of 2 ml plastic syringe.
• The reading will be displayed.
• Note the reading.
5.0 Refractive Index at 25 O C.
Refractive Index determined using previously calibrated Refractive Index meter
Procedure:
• Switch “ON” the Refractive Index meter.
• Placed one drop of distilled water on the crystal and cover with lid zero set.
• Placed the drop of sample on the crystal and cover with lid.
• The reading will be displayed.
• Note the reading.
6.0 Moisture
Analysis of Moisture is carried out using Karl Fischer (KF) titrator.
Procedure:
• Take dried methanol in dry titration vessel of previously calibrated KF titrator.
• Press “START” key.
• Weigh accurately the sample and transfer it to titration vessel.
• Enter weight of sample.
• Record your results.
7. Formic acid in DMF (Acidity):
Procedure:
• Weigh accurately about 10gms of DMF.
• Add few drops of methyl blue indicator.
• Titrate against 0.02N KOH solution.
• End point yellow to blue/green.
• Calculation: B.R. x N KOH x 0.045/ wt. of the sample.
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8. DMA in DMF:
Procedure:
• Weigh accurately about 10gms of DMF.
• Add methyl blue indicator.
• Titrate with 0.02N perchloric acid.
• End point is blue/green to yellow.
• Calculation: B.R. x N HClO4 x 0.045/ wt. of the sample.
9. Methanol and DMAC in DMF.
Analysis of methanol and Dimethyl formamide is carried out using previously calibrated gas
chromatographic technique with flame ionization detector (FID)

Chromatographic conditions
• Oven temperature: 110OC for 0.5 min, ramp rate 5 OC/ min up to 180 OC.
• Column: Capillary column DB-1. • Hydrogen flow: 70ml/min,
• Injector temperature: 220 OC • Airflow: 300 ml/min
O
• Detector temperature: 250 C
• Carrier gas flow: 40ml/min
• Elution order is CH 3 OH, DMF, and DMAC.
Procedure for Methanol and DM AC in DM F:
• Inject 1µ l of sample in GC on previously calibrated of desired standard.
• Match the retention time with the help of software.
• Calculate concentration of component using respective RF.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
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ANALYSIS OF DMAC:
Analysis of dimethyl acetamide samples in process and finished products is carried out
regularly to ensure specified quality of the product. The samples are tested for different
parameters as follows,
Sr.
No. Test Specifications.
1 APPEARANCE CLEAR & FREE OF SUSPENDED SOLIDS
2 COLOUR ( APHA ) < 10
3 pH 20 % aqueous solution 4 TO 5
5 CONDUCTIVITY < 40
6 DENSITY GM/CC AT 20 DEG. C. 0.935 – 0.942
7 REFRACTIVE INDEX AT 25 DEG. C. 1.4358 – 1.4360
8 WATER ( % ) 0.05 MAX
9 ACETIC ACID ( % WT ) 0.1 MAX
10 PURITY (% WT MIN.) 99.75
1. Color and appearance
The sample shall be colorless and free from suspended material. Analysis of Color and
appearance is carried out using Spectrophotometer or Nessler’s tube.
Procedure:
• Read operating instructions from spectrophotometer manual.
• Load method file (i.e. meant for APHA) from the file menu of spectrophotometer.
• Use distilled water as blank and 10mm path length cell.
• Load the given sample to find out APHA value by using previously calibrated
spectrophotometer for APHA Method.
• Record the result. ( APHA)
• Alternately the same can be measured by taking desired different APHA standards in
Nessler’s tube and match the sample color.
• Report the matched one standard as result ( APHA)
2. pH of 20% DMAC solution:
pH is carried out using previously calibrated pH Meter.
• Take 20ml of dimethyl acetamide.
• Add 80ml of distilled water & stir.
• Measure the pH
3. Conductivity of 20% DMAC solution:
Conductivity is carried out using previously calibrated Conductivity Meter.
• Take 20 ml of dimethyl acetamide.
• Add 80ml of distilled water & Stir.
• Measure the conductivity.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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4. DENSITY at 20O C
Density determined using previously calibrated density meter.
Procedure:
• Switch “ON” the Density meter.
• Introduce the sample with the help of 2 ml plastic syringe.
• The reading will be displayed.
• Note the reading.

5. Refractive Index at 25 O C.
Refractive Index determined using previously calibrated Refractive Index meter
Procedure:
• Switch “ON” the Refractive Index meter.
• Placed one drop of distilled water on the crystal and cover with lid zero set.
• Placed the drop of sample on the crystal and cover with lid.
• The reading will be displayed.
• Note the reading.
6. Moisture
Analysis of Moisture is carried out using previously calibrated Karl Fischer (KF) titrator .
Procedure:
• Take dried methanol in dry titration vessel of the previously calibrated KF titrator.
• Press “START” key.
• Weigh accurately the sample and transfer it to titration vessel.
• Enter weight of sample.
• Record your results.
7. Acetic acid in DMAC (Acidity):
Concentration of acetic acid in different samples of the plant and finished product is analyzed
titrimetrically.
Procedure:
• Weigh accurately about 10gms of DMAC.
• Add few drops of phenolphthalein indicator.
• Titrate against 0.02N NaOH solution.
• End point colorless to pink
• Calculation: B.R. x N KOH x 0.060/ wt. of the sample.
9. Excess Acetic acid in R003: In-Process samples
• Weigh accurately about 0.2 gms of sample.
• Add phenolphthalein indicator.
• Titrate with 0.2N sodium hydroxide.
• End point is color less to pink.
• Calculation: B.R. x N HCl x 0.060X 100 / wt. of the sample.
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10. Excess DMA in T12: in Process samples

• Weigh accurately about 0.2 gms of sample.
• Add bromothymol blue indicator.
• Titrate with 0.2N hydrochloric acid.
• End point is blue/green to yellow.
• Calculation: B.R. x N HCl x 0.045X 100 / wt. of the sample.

11. MMAC and DMAC in R003 In-Process samples.

Analysis of methanol and Dimethyl acetamide is carried out using previously calibrated gas
chromatographic technique with flame ionization detector
Chromatographic conditions
• Column: Capillary column DB-1.
• Oven temperature: 80OC. • Final Time 8 Min.
• Initial time : 0.2 min • Injector Temp: 200 OC
O
• Ramp rate 1 : 20 C • Detector : FID
• Final Temp: 100OC • Detector Temp: 250 OC
• Final Time: 4 Min. • Carrier N2 :40ml/min
• Ramp rate 2 :20OC • Hydrogen: 70ml/min,
O
• Final Temp: 180 C • Air Flow : 300 ml / min
• Elution order is MMAc, DMAc.
Procedure:
• Appropriately dilute R003 sample with water and note the dilution factor.
• Inject 1µ l of above diluted sample in gas chromatograph on previously calibrated of
desired standard.
• Match the retention time with the help of software.
• Calculate concentration of component using respective response factors and
multiply by dilution factor.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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FORMIC ACID:

Sr.
No. Test Specifications.
1 APPEARANCE CLEAR
2 COLOUR ( APHA ) < 50
3 Chloride 0.003% Max
4 Sulfate 0.003% Max
5 NVM 0.008% Max
6 PURITY 99.85 % Wt Min

Analysis of in process and finished product Formic acid plant samples is carried out regularly
to ensure specified quality of the product.
1. Color and appearance
The sample shall be clear. Analysis of Color and appearance is carried out using Nessler’s
tube.
2. Chloride:
Procedure:
• Dissolve 10 ml of sample in 30 ml distilled water.
• Add 5 ml 5N Nitric acid and 1 ml of 10% AgNO3.
• Dilute with distilled water to 50ml. Measure the turbidity.
• Compare with the standard solutions of Chloride.
3. Sulfate:
Procedure:
• Take 10 ml of sample add 0.2 mg Sodium Carbonate.
• Evaporate to dryness.
• Dissolve the residue in 40 ml distilled water
• Add 10 ml of ethanol.
• 1ml of 5N HCN and add 1 ml BaCl2 (10%).
• Stand for 1 hour. Measure the turbidity.
• Compare with the standard solutions of Sulfate.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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4. Concentration Purity:
Concentration of formic acid in different samples of the plant and finished product is analyzed
titrimetrically.
Procedure:
• Take 0.2 to 0.25 gms. of sample,
• Titrate against 0.2 N NaOH using phenolphthalein indicators.
• End point is colour less to pink.
• Calculate % formic acid as follows,

Where: 4.6 is factor for Formic Acid.

BRNaoH is Burette Reading of sodium hydroxide.
NNaoH is Normality of sodium hydroxide.

5. Non volatile matter (NVM)

Procedure:
• Take the weight of empty dry 100 ml evaporating dish as W1.
• To this add sample and weigh it as W2.
• Evaporate to dryness on water bath. Cool the evaporating dish in a descicator.
• Take the weight of cool evaporating dish as W3.
• Calculate % NVM as follows.
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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METHYL FORMATE: SPECIFICATIONS :

Sr.
No. Test Specifications.
1 Methyl formate % Min 95.0
2 Methanol % Max 5.0
Methyl formate is analyzed on gas chromatograph having thermal conductivity detector.
Typical gas chromatograph conditions are

Chromatographic conditions
• Column: Porapack–QS
• Oven temperature: 90OC. • Injector temperature: 150OC
• Initial time : 5 min • Detector temperature: 150OC
• Ramp rate : 5OC • Current (TCD): 125 mA
• Final Temp: 150OC • Carrier gas flow: 30ml/min (H2)
• Final Time 20 Min.
• Elution order is H 2 O,CH 3 OH,MF, FA

Procedure:
• Inject 1microlit sample in GC on previously calibrated with desired standard.
• Match the retention time with the help of software.
• Calculate concentration of component using respective RF.
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C) HEAVY WATER LAB.

D/D+H:
• Analysis of synthesis gas from HWP & Ammonia plant and condensate samples
from WTP & Ammonia plant for deuterium content is carried out using mass
spectrometer.
• Standardize the instrument with two known lower ppm standards & higher
concentration standards. ( developed departmentally).
• Range 20 to 120 ppm & 1.0% to 1.35%
• Inject few micro litres of sample by glass ampoule & glass syringe on two Mass
Spectrometers.
• Record the D/H ratio with the help of computer. Record in shift analysis log book.
Report to Control to control room.

MOISTURE IN Liquid AMMONIA :

• A : Collect 100 ml of the liquid ammonia in specially fabricated glass apparatus

for 0.1 to 2 % of moisture.
• Evaporate ammonia completely at room temp.
• The residual water remains at the bottom which is calibrated from 0.1 to 2.5 ml.
• From this volume ppm or % of ammonia can be calculated.
• B : Collect about 200 ml ( W gms) of the liquid ammonia in glass reagent
bottle
(Cap. 500 ml) fitted with specially fabricated Glass sample head for the ppm range.
• Keep on adding Potassium wire piece till blue colour persist for atleast 1 minute
(w gms).
• Moisture in ammonia ( ppm) – ( w / W X 18/39) X 100

AMIDE ANALYSIS –Ammonium Bromide & Absorbtion Method.

Absorption method. :
• Amide concentration upto 100 gms/kg of ammonia can be analysed by
Ammonium Bromide Method.
• Collect 25 to 30 gms of Amide sample in Specially designed Glass Ampoule by
using Dry ice Acetone bath.
• Absorb Ammonia vapours in Sulphuric acid till residue of amide remains in
ampoule & ammonia is back titrated against Sodium Hydroxide.
• Then Residue is dissolved slowly by distilled water.
 DEPARTMENTAL IMS MANUAL
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• Once again ammonia present in residue is absorbed in sulphuric acid & back
titrated against Sodium Hydroxide.
• The Potassium hydroxide formed after dissolving the residue is titrated against
Acid.
• Amount of Ammonia in gms. ( say X ) : ( ml of Sulphuric acid X 17.03 / 1000 )
• Amount of Amide in gms. : ( ml of Sulphuric acid x 55 / X )
• Amount of Amide & KOH in gms. ( say Y ) : ml of Sulphuric acid X 56 / X
• Amount of KOH in gms. : X - Y
Ammonium Bromide Method :
• Collect 200 gms ( say P ) of Amide sample in Glass Bottle fitted with sample
head.
• Add pinch of Phenolphthalein Indicator & add Ammonium Bromide till pink end
point. Note down Amount of Ammonium Bromide ( W gms ).
• Put Potassium wire to have a blue colour for at least 1 minute .
• Thus potassium is added to the known weight of sample say Y grams.
• Amount of KOH in gms. ( say Z ) : ((Y x 56/39)) x 1000 / P
• Amount of Amide in gms. : (((W x 55/98) x 1000) / P ) - Z
Potassium Ion in liquid Ammonia :
• A known weight of liquid ammonia is collected
• The sample is evaporated at room temp in from plant at various sample points as
per request from shift incharge.
• The sample is evaporated at room temp in a water bath kept in fume cupboard.
• The contents are washed with 10% dil. HCl and make up to 100 ml in standard
volumetric flask.
• A calibration curve is drawn with 2,5,10 and 20. microgram/ml of potassium
using Flame photometer.
• The sample is introduced and reading obtained, the flame photometer operating
under same conditions.
• Taking in to account the dilution factor and the weight of the sample , the
potassium ion content in liquid ammonia can be calculated.
• Potassium in liquid Ammonia in ppm :
• (Reading for Sample X Std. used X Dilution factor) / (Wt of sample X Reading
for Standard )
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Analysis of Off grade Heavy water :

• A heavy water sample from 18 unit is analysed on Density meter.
• Inject 1 ml of sample in quartz tube of Density meter.
• Adjust the temperature at 25degC. Take Direct reading of Density ( say D ) .
• Calculate the purity.
• % purity - (((D X 10.279428)-(10.249462))/(0.999973 X D )) X 100
Analysis of Nuclear grade Heavy water.:
• Collect heavy water sample in dried glass flat bottom flask.
• Analyse it on FTIR as per WI /QCL/03.
• Switch on FTIR.
• Scan the instrument for background scan.
• Fill the 0.2 mm CaF2 window cell by Heavy Water Sample.
• Record the absorbance against wavelength ( 3350 to 3450 nm ) by built in
software. Calculations are done with the help of quantification software.
• Store the graph in Computer.
• Calculate the purity of the sample by software or manually.

Analysis of Reject from 25 unit. :

• A reject water sample from 25 unit is analysed on Density meter.
• Inject 1 ml of sample in quartz tube of Density meter.
• Adjust the temperature at 25degC.
• Take Direct reading of Density.
• Calculate the purity.
• % purity - (((D X 10.279428)-(10.249462))/(0.999973 X D )) X 100
Oxygen content at trapper outlet.
• Collect a sample in bladder.
• Inject the sample on Gas Chromatograph in central lab. ( WI/QCL/03)

Moisture content in synthesis Gas :

Put on the instrument. Flush the sample for some time. Then adjust flow at 2 lits/min.
Then take direct reading of dew point on instrument. Calculate moisture.

Oil samples from Lube oil tank: Analyze moisture by putting one drop of oil on hot
plate. If cracking is observed, the test is said to be positive & moisture present. If test is
negative, moisture is said to be NT. Refer work instruction of central lab.
 DEPARTMENTAL IMS MANUAL
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D) WATER TREATMENT LAB.

MIDC raw water, WTP I (Thermax), WTP -II (BPMEL) and settler water from Ammonia
plant is analysed for pH, Conductivity,Hardness, M-Alkalinity, P-Alkalinity, Silica,
Carbon dioxide, free mineral acidity and turbidity.
Sample Points :
WTP - I (Thermax) –

Anion A,B & C

MB A,B & C

DM Tank

Degasser

Cation A,B & C

WTP-II (BPMEL) -
• Anion 1,2 & 3
• MB 1,2 &3
• PMB 1, 2 & 3
• DM Tank
• Degasser
• Cation 1,2 & 3

STEAM GENERATION PLANT :

Samples from Boilers and Turbo Generators are analysed for pH, Conductivity, P-
alkalinity, Hardness, Chloride, Hydrazine Hydrate and silica.
Sample Points :
• Super heater steam I, II & III
• Saturated steam I, II & III.
• TG I & II

DA 501 & 502.

Ammonia condensate

urea condensate

V2-P18 Tank

V2

P18 line
 DEPARTMENTAL IMS MANUAL
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TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ANALYSIS OF COOLING, PROCESS , BOILER AND EFFLUENT WATER. :

The analysis of cooling, process, Boiler and effluent water is carried out regularly. The
cooling water is analyzed for pH, conductivity, turbidity, total hardness, calcium
hardness, M-alkalinity, P-alkalinity, phosphate, chloride, dispersant, iron, zinc , silica
and dissolved oxygen etc.
Check Calibration for instruments as per WRK/QCL/03.
Process Water :
pH : Measure the pH on pH meter.Ref. WRK/QCL/01.
Conductivity :
• Measure the conductivity on conductivity meter.Ref. WRK/QCL/01.
COLLOID SILICA :
• Take 50 ml of sample add 0.2 gms of sodium bicarbonate in a clean platinum
dish.
• Digest it on hot plate till it is reduce to half volume.
• Cool the sample at R.T. And add 2.4 ml of 1.0 N sulphuric acid to neutralize the
digested sample. Then take the reduced sample in to the 100 ml Nessler glass
tube and make up with washing the platinum dish with appropriate sample to 50
ml.
• Similarly run blank sample with DW. Then add 2 ml of acidic ammonium
molybdate.
• Wait for 4 minutes, then add 4 ml of 10 % Oxalic acid and after some time add 1
ml of metol.
• Wait some time and measure silica on silica standard file on spectrophotometer.
• This will be our total silica.
• Measure the reactive silica as usual method.
Calculation :
Colloid or non reactive silicain ppm = (Total silica - reactive silica)
Silica :
Reagents.
• Acid ammonium molybdate ( 5%)
• Oxalic acid (10%)
• Metol solution
Procedure:
• Take 50 ml sample in nessler tube . Add 2 ml of acidic ammonium molybdate, 4
ml 10 % oxalic acid and 1 ml metol solution.
• Shake well and wait for 5 minute after each addition.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 28 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

• Shake well and allow the colour to develop for about 10 minute. Blue colour will
developed. Prepare blank and take reading on spectrophotometer
Phosphate :
Reagents :
• Nitric acid 1:!
• Ammonium molybdate 10 %
• Acidic ammonium vanadate
Procedure:
• Take 25 ml sample in conical flask . Add 5 ml 1:1 HNO3 .
• Digest for 20 minute.
• Cool, add 5 ml each of 10% Ammonium molybdate and Ammonium vanadate.
• Make up to 50 ml. Shake well and allow the colour to develop for about 15
minutes.
• Prepare blank and take reading on spectrophotometer
Free mineral acidity & carbon dioxide :
Procedure:
• Take 50 ml of sample + 2 drops of M.O.indicator and titrate against 0.02 N NaOH
solution. Reading × 20 will be F.M.A. Then take 50 ml of sample + 2 drops of
phenolphthalein indicator and then titrate it with 0.02 N NaOH Solution.
• Colorless to pink will be the end point.
CO2 Calculation :
(P-reading − M-reading ) × 20
P-Alkalinity :
Reagents :
0.02 N HCl
• Take 100 ml of sample in 150 ml clean & dry beaker.
• Add few drops of Phenolphthalein indicator and titrate against 0.02 N HCl
solution. till color changes from pink to colourless.
Calculation :
P-Alkalinity as CaCO3 ppm = ( Rd. x N of HCl x 50 x 1000 ) / ml of sample
M-Alkalinity :
Reagents :
0.02 N HCl
• Continue the titration of P-Alkalinity by add few drops of Methyl Orange indicator
till color changes from yellow to orange.
Calculation :
M-Alkalinity as CaCO3 ppm = (Rd. x N of HCl x 50 x 1000) / ml of sample.
Hydrazine Hydrate :
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 29 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Reagents :
• 0.2 N HCL
• P-Diamethyl amino benzaldehyde
• Standard Hydrazine solution
Procedure:
• Take 50 ml sample in nessler’s tube.
• Add 2 ml 0.2 N HCL and 5 ml P-Diamethyl amino benzaldehyde.
• Also prepare reagent blank. Take reading on spectrophotometer at wavelength
458 nm.
Dissolved Oxygen :
Reagents :
• MnSO4
• KI + KOH
• Conc. H2SO4
• Sodium thio-sulphate
• Starch indicater
Procedure:
• Take 500 ml air tight sample in iodine flask.
• Add 2 ml of each MnSO4, KI + KOH and Conc. H2SO4 .
• Precipitate formed by adding KI + KOH get dissolved in sulphuric acid.
• Yellow colour appears .
• Titrate this against 0.025 N Sodium thio Sulphate using starch as an indicater.
• End point is blue to colourless.
Calculation :
PPM OF D.O : ( Reading X 0.2 X 1000) / sample volume
Iron:
Reagents:
• HCL 1:1
• KSCN 10 %
• Std. Iron solution ( 1ml = 0.1mg of iron)
Procedure:
• Take 50ml sample in Nessler’s tube.
• Add 2ml 1:1 HCL and 5ml 10 % KSCN. Also prepare blank.
• Allow the color to develop for about 10 to 15 min. Measure the concentration on
spectrophotometer at wavelength 410nm
WASTE WATER :
P18 is tested for pH, Conductivity, Silica, Ammonia and Urea
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 30 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

V2 condensate is tested for pH, Conductivity, Silica and Ammonia.

Turbidity :
• Turbidity of sample is measured on turbidity meter.
• Check calibration as per WRK/QCL/03.
• Take distilled water in turbidity meter tube. adjust the zero of the instrument with
water.
• Shake the sample well before transferring to the tube. Note the reading.
Total hardness:
• Total hardness is determined by titrating sample with standard EDTA solution.
• Take 50ml of sample, add 2ml of pH 10 buffer solution. add a pinch of Erichrome
black T indicator.
• Titrate against 0.01M EDTA from pink- violet to blue end point
TH in ppm = BR x 20
Calcium hardness :
• Calcium hardness is determined by titrating water sample with standard EDTA
solution.
• Take 50ml sample+ 2ml of pH 10 buffer.+ a pinch of murexide indicator.
• Titrate against 0.01M EDTA solution, end point purple to violet.
CaH in ppm = BR x 20
Chloride :
• Chloride content in cooling water is determined by titrating the sample with
standard silver nitrate solution.
• Take 50ml of sample, Adjust the pH between 7 – 7.5 with dilute sodium
hydroxide and dilute nitric acid.
• If the sample contains excess of ammonia boil the sample to ensure that
ammonia is removed. This is necessary as ammonia interferes in the estimation
of chloride.Add few drops of 5% potassium chromate indicator.
• Titrate against std. 0.01N AgNO3 yellow to hazy reddish brown end point.
• Take a blank reading with distilled water
Chloride in ppm = BR(B)-BR(F) x 9.2
Record the result in all labs. & report to shift in charge telephonically followed by
detailed report
Dispersant :
• Dispersant in cooling water is determined by titrating the sample with standard
thorium nitrate solution.
• Take 50ml sample, adjust the pH of soln. between 3 – 3.5 with dil. nitric acid.Add
few drops of 0.01% xylenol orange reagent.
• Titrate against 0.005N std. thorium nitrate yellow to yellowish brown end point.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 31 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

• End point is yellow to yellowish brown.

Dispersant = BR(B) - BR (S) x 33.25
Iron :
• Iron in cooling water reflects the corrosion due to various factors.
• Iron in cooling water is estimated photometrically at 480nm.
• 50ml sample + 2ml 1:1 HCl +5ml 5%Ammonium Persulphate+ 5% KSCN
• Adjust absorbance on the spectrophotometer to zero with reagent blank.
• Place sample in cuvette and measure absorbance & concentration of sample.
Phosphate:
• Phosphate content in C.W. is determined photometrically .
• Take 50ml of sample + 2ml 1:1 nitric acid,Digest on hot plate.Cool & transfer in
50ml Nessler’s cylinder.
• Add 5ml 10% ammonium molybadate soln.+ 5ml of pot. Metavanadate soln
• Make up to 50ml with distilled water. Prepare reagent blank & adjust the zero of
the instrument. Placing the sample in cuvette, measure the abs / concn. of the
phosphate.

Ammonia:
Reagents:
• 0 .2N HCl
• Mixed indicator
Procedure:
• Take 10ml sample in conical flask.
• Add 2-3 drops of mixed indicator.
• Titrate against 0.2N HCl.
• End point is Green to pink color.

Calculations:
R x NHCl x 0.017 x 100 x 1000
% Total NH3 = -----------------------------------------
Wt. of sample x 10
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 32 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.216

E ) EFFLUENT TREATMENT LAB.

TOTAL AMMONICAL NITROGEN:
• Collect 100 ml sample In kjeldah”s flask take add 25 ml Borax borate buffer &
• 6 N NaOH till pH 9.5 then add glass beeds to 250 ml with D.M. water and distilled it
out.
• Collect distillate in 2% 50 ml boric acid & 50 ml D.M.water then add 4 drops of mixed
indicator.Distillate turns red to green.
• Then titrate distillate with 0.02 N H2SO4.
• End point green to red.
• Note burette reading – R,
• Perform the same exercise for D.M.water as blank.
Calculation:-
= (R – Blank reading X 14 X N of H2SO4 X1000) / Sample volume
Reagent:
• 2% Boric Acid
• 20gms of Boric Acid dissolve in 1000ml D.M.water.
• Borax Borate Buffer – 88ml 0.1 N NaoH+500ml .025N Na-tetra borate
• 9.5gm Na-tetra borate to1000ml (.025N) + 2gms to 500ml (0.1N)

TOTAL ORGANIC NITROGEN :

• In remaining residue of total ammonical nitrogen add 6.7 grams of K2SO4, 1.5 grams
of HgSO4, 10 ml concentrated H2SO4 & glass beeds
• After mixing heat under hood to remove SO3 fumes about 30 minutes.
• Cool it .then dilute it to 300 ml with D.M. water.
• Then add 0.5 ml phenolphthalein. And mixed it then add 50 ml Thiosulphate hydroxide
to form alkaline layer.
• Connect the flask (colourless to pink ) for distillation.
• Distilled collection is collected in flask with 50 ml 2% Boric acid, 50 ml D.M. water.
• Then add mixed indicator, then titrate it with 0.02 N H2SO4.

Calculation:
T.O.N. = ( Sample reading – blank reading X 280) / Sample volume

T.K.N.= ( T.A.N. + T.O.N. )

Reagent:
Thiosulphate Hydroxide – Disslove 500gms NaOH +25gms Na2s2O5, 5H2O Dilute to 1
Litre.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 33 of 34
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APPROVED BY: HOD EFFECTIVE DATE: 10.05.216

NITRATE NITROGEN (NO3- N )

• In remaining residue of total ammonical nitrogen add 1 gram of devardes alloy and
sufficient quantity of D.M. water up to 350 ml.
• Distilled out and collect the distillate in flask with 2% Boric acid, 50 ml D.M. water.
• Titrate it with 0.02 N H2SO4
Calculation:
Sample reading – Blank reading X 280 / Sample volume
Reading X 2.8 = ppm.

DISSOLVED OXYGEN :
Full bottle technique
• Collect full volume sample remove air bubbles add 2ml MNSO4. Shake (wait for two
minutes ). Then add 2ml KI – KOH shake (wait for two minutes ), add 2ml
Concentrated H2SO4 shake (wait for two minutes ) reddish yellow colour appears
transfer the material to 500 ml beaker + glass rod add 1ml starch indicator turn blue.
• Titrate with 0.1 N Na2S2O3 till colourless
Calculations:
D.O. = reading X normality X 8 X1000 / Sample volume
Solution Preparation- (KI – KOH)
• 150gms of KI + 700 gms of KOH make to 1 litre.
• MnSo4 – 350 gms of MnSo4 make to 1 litre.
• Strach Indicator - 1gms of starch dissolve in 100ml D.M. Water .
Chemical oxygen Demand. ( C.O.D.)
• Chemical oxygen of the sample is determined by C.O.D. monitoring instrument.
• Samples from different plants are analysed on the instrument.
• Record the results.
Bio- chemical oxygen Demand. ( B.O.D.)
• Chemical oxygen of the sample is determined by B.O.D. monitoring instrument.
• Samples from different plants are analysed on the instrument.
• Record the results.

Main effluents generated from All plants are analysed in respective plants.
A) CENTRAL LAB.
• Effluent sample from Ammonia & urea plant is analyzed for Ammonia.
• Analyze the sample as per procedure given in cooling water analysis.
B) CHEMICAL GROUP LAB.
• The common liquid effluents of MAP (Old & New plants), DMF and DMAC plants are
collected from the sample point in Methyl amine plant (old).
• The common liquid effluent is analyzed for pH, Conductivity, Turbidity & M. Alkalinity.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: ANALYSIS OF PROCESS SAMPLES AND FINISHED PRODUCT.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 34 of 34
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.216

• Sampling and Analytical Techniques:

• Total Suspended Particulate Matter TSPM, RPM, SO2 and NOx
• Suspended Particulate Matter present in ambient air is drawn through the cyclone.
Coarse and non- respireable dust is separated from the air stream by centrifugal forces
acting on the solid particles. These separated particulates fall through the cyclone's
conical hopper and collect in the sampling cup placed at the bottom of the cyclone. The
fine dust forming the respirable fraction passes the cyclone and is retained by the filter
paper. The TSPM is estimated by summing up the SPM and RPM fractions collected
separately as above.
• A tapping is provided on the suction side of the blower to provide suction for sampling
air through a set of impingers. Samples of gases are drawn at a flow rate of 1.73 Liters
per Minute (LPM).
• TSPM and RPM have been estimated by Gravimetric method, spectrophotometer
methods for estimation of SO2, NOx and ammonia has been adopted for the
estimation.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-03
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 7
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

INTRODUCTION
• Calibration of laboratory instruments is important for accuracy, precision and reliability of
analysis.
• Calibration of laboratory instruments is carried out at regular intervals to keep instruments
in good working conditions.
1. Calibration of pH meter.
• Read the operating and calibration instructions from the user manual.
• pH meter is calibrated by using buffer solutions of pH 4,7 and 9.
• The preparation of buffer solutions is described in QCL/WRK/04.
• Following steps standardizes it.
• Select cal mode on the instrument.
• Wash the electrode with distilled water.
• Wipe it with tissue paper.
• Immerse the electrode in the buffer solution of either 4 or 7.
• Press start button to initiate calibration process.
• Enter the current temperature as calibration temperature.
• Enter the value of first buffer solution at calibration temperature.
• The voltage of first buffer at the calibration temperature is measured; when the value has
met the set drift criterion the measurement is stopped.
• The instrument asks for the second value of the buffer.
• Enter the second value of the buffer follow the above procedure.
• At the end of the calibration data obtained is displayed.
• Store the calibration data on the instrument.
• The calibration of the pH meter is done once in two months.
• Prepare fresh buffer solutions before calibration.
• Record the report in TH-IMS/REC/QCL/01.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 7
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

2. Calibration of Conductivity meter.

• Read the operating and calibration instructions from the user manual.
• Conductivity meter is calibrated by using solutions of 0.1 N, 1 N KCl.
• Prepare fresh KCl solution before calibration.
• The preparation of KCl solutions is described in QCL/WRK/04.
• Follow steps of operating and calibration instruction from the user manual.
• The calibration of the conductivity meter is done once in two months.
• Record the report in TH-IMS/REC/QCL/01.
3. Calibration of Karl Fischer titrator
• The Karl Fischer titrator is used to determine moisture content in samples like dimethyl
formamide, methanol, acetic acid, dimethyl acetamide & Urea prills etc.
• The calibration is carried out as described below.
• Select TITRE with water (mode).
• This mode is accepted by pressing enter.
• Now the instrument is in titer mode.
• Check the settings by pressing <Parameter> key.
• Take methanol in titrating vessel.
• Press “start “key, neutralize the methanol.
• Keep the instrument in ready condition by pressing <start> key.
• Weigh accurately 0.01 g of water.
• Transfer the water to titrating vessel.
• Enter the weight of the water by using keypad.
• Press start.
• Titration proceeds to completion.
• On completion the first line of display gives the dispensed volume of Karl–Fischer reagent.
• The second line displays the calculated titer value.
• Repeat the titration.
2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

• On completion of the second titration mean titer value is given.

• Store the titer value on instrument.
• Record the report in TH-IMS/REC/QCL/01.
4. Photometric Accuracy of spectrophotometer
• Scan the Instrument from 200 to 400 nm wave length
• Make zero absorbance by placing 1 cm cell filled with 0.01 N H2SO4 in both the
compartment
• Place the prepared potassium dichromate solution in the reference compartment and take
the absorbance at wavelengths 235, 257, 313, & 350nm respectively.
• Note the absorbance and calculate the extinction magnitude of absorbance.
• E = Absorbance / (gms of potassium dichromate / 10)
• The tolerance limit for particular wavelength is i) 235 nm = 122.9 to 126.2
ii) 257 nm = 142.4 to 145.7 iii) 313 nm = 47.0 to 50.0 iv) 350 nm = 104.9 to 108.20.
5. Calibration of spectrophotometer
• Prepare the ion or radical standard stock solutions to be tested
• Set desired wavelength, absorbance range & the concentration of standards on the
instrument menu.
• Make auto zero for reference blank and then feed the prepared standards serially from zero
to last standard.
• The instrument displays calibration graph on the screen.
• Store the graph on the instrument.
• The ions / radicals tested on the spectrophotometer are iron, phosphate, color, etc.
• Prepare standard graph for each in similar way.
• Use these stored files while analyzing.
• The calibration is carried out once in six months.
• Record the report in TH-IMS/REC/QCL/01.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 7
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

6. Calibration of gas chromatograph

• Read the operating and calibration instructions from the user manual.
• Certified gas standards of reputed supplier with certificate are use. Or
• Appropriate standards are prepared freshly before calibrating the gas chromatograph.
• The detailed procedures of preparation of such standards are described in QCL/WRK/04.
• Set the chromatographic condition for appropriate analysis described in QCL/WRK/01or 02.
• Wait till the conditions are reached. Allow the instrument to stabilize after achieving the
conditions. Inject appropriate quantity of known standard. Press run key.
• Allow the run to complete. Calibrate the GC with the help of provide software with
integrator. Record the report in TH-IMS/REC/QCL/01.
7. Calibration of balance
• Balance is calibrated by following steps,
• Switch on the balance, Press tare bar and hold.The instrument passes through series of
steps to complete the calibration. Check the calibration by weighing 100g weights for at
least five times. Note readings; subsequently find out the variation in readings by taking
average weight.
• Record the report in Calibration record file.
• Balances of all laboratories are calibrated quarterly by external agency & weight box is
calibrated yearly by external agency at their works.
8. Calibration of Density meter
• Switch on the density meter.
• Switch on the pump and purge the instrument with air.
• Then clean the instrument tube with ultra pure water.
• Then dry the instrument with air. Inject ultra pure water in the instrument and observes
density at different temperatures.
• Record the report in TH-IMS/TH-IMS/REC/QCL/01.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 5 of 7
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

•
9. Calibration of Refractometer
• Make the Instrument on and clean the prism properly with tissue paper.
• Put extra pure distilled water on prism; take reading at 10°C to 50°C.
• If the readings are not matching with the standard values, adjust the reading.
• The instrument is having built calibration.
• Instrument to be calibrated once in two months.
• Find the Refractive Index of any unknown sample.
• Record the report in TH-IMS/TH-IMS/REC/QCL/01.
10 Calibration of Nephelometer
• Switch on the Nephelometer
• Set the instrument for zero by using distilled water.
• Then adjust the turbidity value i.e. NTU by using standard turbidity solutions. i.e. 40 NTU &
10 NTU.
• Record the report in TH-IMS/TH-IMS/REC/QCL/01.
11. Calibration of Digital Burette
• Measure 50 ml distilled water from burette. Weigh the same volume. Note the reading.
• Perform the same exercise five times.
• From data, calculate Mean Value, Mean Volume,
• Standard Deviation, Accuracy & coefficient variation (CV).
• Accuracy (%) = Mean Vol. - Reading/ Reading X 100.
• CV ( % ) = Standard Deviation X 100 / Mean Volume
• Record the report in TH-IMS/TH-IMS/REC/QCL/01.
12. Mass Spectrometer:
• Inject 0.1 micro lit of gas standard in Mass Spectrometer No. 1 sample Inlet system.
• Then record the Ratiometer reading calculated by software.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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APPROVED BY: HOD EFFECTIVE DATE: 01.12.2012

• Use two no. of gas standards ( in house generated) for lower range. Plot the graph by using
software.
• Same procedure is followed for Higher concentration deuterium standards in Mass
Spectrometer No. 2
• Record the report in TH-IMS/REC/QCL/01.
13. FTIR:
• Switch on FTIR; Scan the instrument for background scan.
• Fill the 0.2 mm Caf2 window cell by Heavy Water Standards (Standards Ranging from
99.86 % to 99.96%).
• Scan the instrument for all Standards.
• Plot the graph of Absorbance against wavelength by built in software.
• Calculations are done with the help of software.
• Store the graph in Computer.
• Then inject the sample in same cell for absorbance & calculate the purity of the sample.
• Record the report in TH-IMS/REC/QCL/01.
14. Flame Photometer:
• Put on the instrument.
• Put on the air flow.
• Light the burner and adjust the Flame.
• Calibrate the instrument by aspirating 1 ppm and 4 ppm of Potassium standards.
• Results are obtained by aspirating sample.
16. Dew point meter. :
Dew point meter is having self calibration mode. Put on the dew point meter. Flush the sample
for some time. Adjust flow at 2 lts. Per min. Take direct reading of dew point meter.
18. Tensile Bag testing Machine:
• Calibration is done by external sources.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: CALIBRATION OF LABORATORY INSTRUMENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 7 of 7
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• Record the report in TH-IMS/REC/QCL/01.

19. Viscosity meter:
• Calibration is done by using in house secondary standards.
• Record the report in TH-IMS/REC/QCL/01.
20. Calibration of Foss nitrogen analyzer:
• Read the operating and calibration instructions from the user manual.
• Follow steps of operating and calibration instruction from the user manual.
• Put on the instrument.
• Put on the water flow.
• Check nitrogen content of pure ammonium ferrous sulphate.
• The calibration of the instrument is done once in six months.
• Record the report in TH-IMS/REC/QCL/01

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

INTRODUCTION:

The preparation of laboratory reagents plays important role in analysis of samples. All
reagents required for analysis must be prepared carefully in distilled water. Preparation
of frequently used reagents is described in this work instruction.

1. Ammonium molybdate (10 %) solution.

• Weigh accurately about 100g of solid ammonium molybdate powder (LR) in clean
dry beaker. Dissolve the solid in warm distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled
water.
• Keep the solution in clean-labeled reagent bottle.

2. Ammonium molybdate (5 %) solution.

• Add 50 ml concentrated Sulphuric acid continuously and constant stirring in
demineralise water.
• Cool it and add 50 gm ammonium molybdate to it.
• Make up to 1000 ml.
3. Ammonium vanadate (0.25%) solution.

• Weigh accurately about 2.5g of solid ammonium vanadate powder (LR) in clean
dry beaker.
• Dissolve the solid in 500 ml distilled water.
• To this add 20ml of concentrated nitric acid previously diluted in 200 ml distilled
water.
• Stir the solution well with help of magnetic stirrer.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled
water.
• Keep the solution in clean reagent labeled bottle.

4. Acid reagent (p18 urea).

• Dilute 200 ml con. Sulphuric acid to 750 ml and add 1 ml of additive solution.

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 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
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APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

5. Additive solution (p18-urea)

• Dissolve 15 gm iron chloride in 1000 ml graduated flask by DEMINERALISE water.

• During mixing of the solution 300 ml phosphoric acid be added.
• Dilute the solution at 1000 ml at room temperature.

6. Buffer ( pH 4.0 ,7.0 and 9.0 ) solutions

• Buffer solutions of pH 4, 7 and 9 are prepared from respective CONCENTRATED

VOLUMETRIC SOLUTION AMPOULE of buffer solutions.
• Dilute a CONCENTRATED VOLUMETRIC SOLUTION AMPOULE solution of
respective buffer in 500ml clean volumetric flask with distilled water. Label the flask.

7. Buffer (pH 4.5) solution.

• Dissolve 200 gm of reagent ammonium acetate in 500 ml distilled water

• Add 250 ml of glacial acetic acid.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean reagent labeled bottle.

8. Buffer (pH 10) solution.

• Take 568 ml of 25% ammonia solution (LR grade) in a beaker.

• Add 70.0 gm of ammonium chloride (LR) transfer the mixture to 250ml cylinder and
make up to 1000 ml mark with distilled water.
9. Barium Chloride ( 10%) solution

• Dissolve 100 gm of barium chloride in 500 ml distilled water.

• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean reagent labeled bottle.

10. Cadmium acetate ( 10%) solution

• Dissolve 100 gm of cadmium acetate in 500 ml distilled water.

• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean reagent labeled bottle.

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TITLE: PREPARATION OF LABORATORY REAGENTS.
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OHSAS 18001 - PAGE NO: 3 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

11. Colour reagent (p18-urea)

• a) Dissolve 1.6667 gm s of diacetyl monoxime in 400 ml water

• b) Dissolve 0.3333 gm of thiosemicarbozide in 400 ml water
• Mix a & b.
• Filter with Whatman no.1 & make to one liter.

12. Copper sulphate (1.5% ) solution

• Dissolve 15 gms of copper sulphate in 500 ml distilled water.

• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean reagent labeled bottle.

13. Dimethyl Amino Benzaldehyde (4 %) solution.

• Dissolve 40 gm of dimethyl amino benzaldehyde in 500 ml distilled water.

• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean reagent labeled bottle.

14. EDTA (0.01M) solution.

• Weigh accurately 3.7225g of di-sodium salt of EDTA in a clean dry beaker.

• Dissolve the salt in distilled water.
• Transfer the solution to 1000ml standard volumetric flask.
• Make up to the mark with distilled water.
• Shake well to homogenize the solution.
• Transfer the solution to 1litre labeled reagent bottle.

15. Hydrochloric acid (1:1 ) solution

• Take 500ml of distilled water in 1000ml clean measuring cylinder.

• Add 500ml of concentrated hydrochloric acid.
• Transfer the acid solution to clean labeled reagent bottle.

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 14
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APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

16. Hydrochloric acid (1N ) Solution

In 1000ml clean volumetric flask take 500ml of distilled water.

• Add 89ml of concentrated hydrochloric acid carefully.
• Dilute to mark with distilled water.
• Alternatively 1N hydrochloric acid can be prepared from CONCENTRATED
VOLUMETRIC SOLUTION AMPOULE.
• However, Read the instruction placed on CONCENTRATED VOLUMETRIC
SOLUTION AMPOULE ampoule for dilution.

NOTE: For 1000 ml of 0.1 N use 8.9 ml concentrated hydrochloric acid.

17. Iodine ( 0.1N ) solution

• 0.1N standard solution is prepared from iodine CONCENTRATED VOLUMETRIC

SOLUTION AMPOULE.
• Transfer contents of the CONCENTRATED VOLUMETRIC SOLUTION AMPOULE to
a clean 500ml volumetric flask.
• Rinse the CONCENTRATED VOLUMETRIC SOLUTION AMPOULE thoroughly.
• Transfer the rinse to volumetric flask and dilute up to the mark with distilled water.

18. Iron (1000 ppm) solution

• Weigh accurately 1g of pure, clean iron wire.

• Transfer this to a clean beaker. To the beaker add 50ml of 1:1 nitric acid to dissolve
the wire. Transfer the solution to 1000ml clean, labeled volumetric flask.
• Dilute to mark with distilled water.
• Use this solution to prepare working standards.

19. KI+KOH solution

• Dissolve 700 gm KOH in 250 ml DEMINERALISE water.

• Dissolve 150 gms KI in 250 ml DEMINERALISE water
• Mix 1.& 2.
• Make upto 1000 ml DEMINERALISE water

4
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 5 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

20. Manganese sulphate

• Dissolve 364 gm. MnSO4 .H2O in 1000 ml DEMINERALISE water.

21. Metol

• Dissolve 20 gm. Metol and 205 gm sodium bisulphate in 1000 ml demineralise water.

22. Methanolic Perchloric acid ( 0.05 N )

• Take 4.3ml of perchloric acid in 1000ml clean, labeled volumetric flask.

• Dilute to mark with methanol.

23. Nitric acid (1:1 ) solution

• Take 500ml of distilled water in 1000ml clean measuring cylinder.

• Add 500ml of concentrated nitric acid.
• Transfer the acid solution to clean labeled reagent bottle.

24. Oxalic acid (10%)

• Dissolve 100 gm. Oxalic acid in 1000 ml DEMINERALISE water

25. Periodic acid (0.1 N )

• Dissolve 45.588 gm of periodic acid in distilled water and make up to 2 liter.

26. Potassium Iodide (25% ) solution

• Weigh accurately 25g potassium iodide in a beaker.

• Dissolve it in distilled water.
• Transfer the solution to 100ml measuring cylinder.
• Make up to the mark with distilled water.
• Transfer the solution to the amber colored reagent bottle.
• Preserve the solution in dark.
• Prepare fresh solution every time acetic acid is tested for formic acid content.

5
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 6 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

27. Potassium Chloride (0.1 M) solution.

• Weigh accurately 7.456 gm of potassium chloride A.R. Grade previously dried at

150°C.
• Cool in desiccators.
• Dilute to 1 liter. It makes 0.01 M KCl.

28. Potassium thiocyanate (10% )solution

• Weigh accurately about 100 g of potassium thiocyanate (LR grade) in clean dry
beaker.
• Dissolve in distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Keep the solution in clean and labeled reagent bottle.

29. Potassium permanganate ( 0.1 N )

• Weigh accurately about 1.5804 g of potassium permanganate (LR grade) in

clean dry beaker.
• Dissolve in distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.

30. Potassium Hydroxide – Alcoholic (0.1 N)

• Dissolve 5.611 gm of KOH in 2 – 3 ml distilled water and make up to 1000 ml with

Absolute Alcohol

31. Phosphate Standard (500 ppm) solution

• Weigh accurately 2.17g of pure, potassium di-hydrogen phosphate.

• Transfer this to a clean beaker.
• Dissolve in distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute up to the mark with
distilled water.

6
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 7 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

32. Sodium hydroxide (1N ) solution

• Weigh accurately about 40g of sodium hydroxide (LR) pellets in a beaker.

• Dissolve the sodium hydroxide in distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Transfer the solution to 1liter labeled reagent bottle.

33. Sodium hydroxide ( 0.2 N ) solution

• Weigh accurately about 8 g of sodium hydroxide (LR) pellets in a beaker.

• Dissolve the sodium hydroxide in distilled water.
• Transfer the solution to 1000ml volumetric flask and dilute to mark with distilled water.
• Transfer the solution to 1liter labeled reagent bottle.

34. Silver nitrate (0.1N ) solution

• Dry freshly powered silver nitrate at 120 deg C for two hours.
• Cool to room temperature in desiccators.
• Weigh accurately 1.6987g of silver nitrate in a dry beaker.
• Dissolve it in distilled water.
• Transfer the solution to 1000ml volumetric flask.
• Dilute to mark with distilled water.
• Alternatively the silver nitrate solution is prepared from silver nitrate concentrated
volumetric solution ampoule.
• This on dilution to 500ml gives 0.1N standard solution of silver nitrate.

35. Sodium hypobromide (0.1 ) solution

• Take 100ml of 0.1N sodium hydroxide in a clean conical flask.

• Add to this with through mixing 2.8ml of liquid bromine.
• Dilute to mark with distilled water.
• Transfer the solution to labeled reagent bottle. Preserve the solution in dark.
• Prepare fresh solution monthly.

7
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
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ISO 14001 -
OHSAS 18001 - PAGE NO: 8 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

36. Sodium hydrogen sulfite (1.25% ) solution

• Weigh accurately 1.25g of sodium hydrogen sulfite in clean beaker.

• Dissolve the salt in distilled water.
• Transfer the solution to a clean 100ml volumetric flask and dilute to mark with distilled
water. Preserve the solution in amber colored reagent bottle.
• Prepare fresh solution every time acetic acid is tested for acetaldehyde content.

37. Sodium thiosulfate (0.1N)

• Sodium thiosulfate is prepared from concentrated volumetric solution ampoule.

• Transfer contents of the CONCENTRATED VOLUMETRIC SOLUTION AMPOULE to
a clean 500ml volumetric flask.
• Rinse the CONCENTRATED VOLUMETRIC SOLUTION AMPOULE thoroughly.
• Transfer the rinse to volumetric flask and dilute to mark with distilled water.
• Sodium thiosulfate is primary standard for volumetric analysis.

38. Sodium thiosulphate (0.025 N)

• Take 500 ml of 0.1 N sodium thiosulfate in 2000 ml volumetric flask and dilute by
demineralise water.

39. Sodium Sulphide ( Na2S ) 10 %

• Dissolve 10 gm of sodium sulphide in distilled water and make up to 100 ml.

40. Sodium Arsenite (0.1 N)

• Dissolve 25.984 gm of sodium arsenite in distilled water and make up to 2000 ml.

41. Sodium potassium tartarate (5%)

• Dissolve 250gm of Na-K tartarate & 200gm NaOH in distilled water and make up
5000ml

42. Sulphuric acid (15 % )

• Take 150 ml concentrated Sulphuric acid in measuring cylinder

8
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 9 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

• Pour 150 ml conc. concentrated Sulphuric acid cautiously in distilled water and make
up to 1000 ml.

43. Sulphuric acid (0.2 N)

• Dilute 200 ml 1 N soln to 1000 ml to make 0.2 N soln.

44. 1:1 Sulphuric acid

• Take 500ml of concentrated Sulphuric acid in 1000ml clean measuring cylinder.

• Add 500 ml distilled water slowly in it.
• Transfer the acid solution to clean labeled reagent bottle.

45. Turbidity Standard ( 400 NTU ) solution

• Preparation of stock solution for turbidity standard

A) Solution:
• Weigh accurately 1gm of hydrazine sulphate in a clean beaker.
• Dissolve the salt in distilled water.
• Transfer the solution to 100 ml volumetric flask.
• Dilute to mark with distilled water.

B) Solution:
• Weigh accurately 10g of hexamethyl tetramine in a clean beaker.
• Dissolve the salt in distilled water.
• Transfer the solution to 100ml volumetric flask.
• Dilute to mark with distilled water.

Transfer the solution to 100ml volumetric flask. Dilute to mark with distilled water. Mix the
50ml of solution (A) with 5ml of solution (B) in a 100 ml volumetric flask. Keep for
overnight. Dilute up to the mark with distilled water.

46. Titration solvent

• 495 ml iso propanol + 5 ml distilled water + 500ml Toluene.

9
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 10 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

47. Thorium nitrate (0.005M ) solution

• Weigh accurately 6.9 gm of pure hydrated thorium nitrate in a clean dry beaker.
• Dissolve the salt in distilled water.
• Transfer the solution to 250ml volumetric flask.
• Dilute to mark with distilled water.
• The resulting solution will have strength of 0.05M.
• This is used as stock solution.
• Take 25ml of thorium nitrate stock solution in clean dry 250ml volumetric flask.
• Dilute to mark with distilled water.
• The resulting solution will have strength of 0.005M

48. Preparation of standard for amines

• In 100ml volumetric flask takes 15 ml of distilled water,

• Weigh the flask, add about 10 ml of 40% mono methylamine solution
• And weigh the flask again.
• Similarly add 10 ml of 40% of dimethyl amine solution,
• 12 ml 30% tri methylamine solution,
• 1 ml of methanol and 1.5 ml of ammonia solution to the flask weigh the flask after
each addition. Note the weights of each constituent on paper.
• The final concentration of each constituent is calculated.
% MMA = Wt. of MMA x conc. of MMA solution /100
% DMA = Wt. of DMA x conc. of DMA solution /100
%TMA = Wt. of TMA x Conc. of TMA solution /100
% Ammonia = Wt. of Ammonia x Conc. of Ammonia solution /100
% Methanol = Wt. of Methanol x Conc. of Methanol /100

10
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 11 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

49. APHA Standard for 500 APHA

• Weigh accurately 0.623 gm of chloropalatinate and 0.5 gm cobaltus chloride hexa

hydrate in a clean beaker to this add 50 ml concentrate hydrochloric acid warm it.
• Transfer the solution to 500 ml volumetric flask.
• Dilute to mark with distilled water.

50. Potassium carbonate ( K2CO3 ) 15 %

• Dissolve 15 gm of Potassium carbonate in distilled water and make up to 100 ml.

50. 12.5 N H3PO4

Take 275 ml phosphoric acid and dilute to 1000 ml

51. 10.5 N KOH

Weigh accurately 588 gm of potassium hydroxide and dilute to 1000 ml with

distilled water.

52. STD GV Solution.

36 gm K2CO3 + 1.2 gm Glycine + 0.50 gm V2O5 dilute to 100 ml volumetric flask.

53. Hydroxyl amine hydro chloride : 2 %.

• Dissolve 2 gms of Hydroxyl amine hydro chloride in distilled water and make up to
100 ml.

54. Potassium std. for flame photometer ( 100 ppm) : Standard for potassium content
can be prepared by Potassium Chloride ( 112.1 gms.) dissolved in 1000 ml of
distilled water.

11
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 12 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

INDICATORS:
The preparation of indicators plays important role in analysis. Preparation of frequently
used reagents is described in this work instruction.

1) Bromothymol blue (0.1%)

• The indicator is used for determination of amine concentration of methylamines plant.

• Weigh accurately 0.1g of bromothymol blue indicator in a beaker.
• Dissolve the indicator in ethanol with constant stirring.
• Transfer the solution to 100ml volumetric flak and dilute to mark with ethanol.
• Transfer the indicator to labeled indicator bottle.

2) Erichrome black T

• This indicator is used for determination of total hardness of water.

• The indicator is used in powered form, as the solution is not stable.

3) Muroxide

• This indicator is used for determination of calcium hardness of water.

• The indicator is used in powered form, as the solution is not stable.

4) Methyl red 0.1%

• The indicator is used in acid base titrations.

• Weigh accurately 0.1g of Methyl red indicator in a beaker.
• Dissolve the indicator in ethanol with constant stirring.
• Transfer the solution to 100ml volumetric flak and dilute to mark with ethanol.
• Transfer the indicator to labeled indicator bottle.

5) Mixed indicator

• A mixture of equal parts of 0.1% of methyl red and methylene blue is dissolved in
ethanol.
12
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 13 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

• The end point is blue to green.

6) Mixed indicator

• A mixture of equal parts of 0.1% of bromocresol green and methyl red is dissolved in
ethanol is mixed in the ratio of 2:1.
• The end point is green to red.

7) Methyl orange 0.1%

• Weigh accurately 0.1g methyl red indicator in a beaker.

• Dissolve the indicator in water. Transfer the solution to 100 ml volumetric flak.
• Dilute to mark with distilled water.
• Transfer the indicator to labeled indicator bottle.

8) Phenolphthalein 0.5%

• The indicator is used for determination of alkalinity in cooling water and in acid base
titrations.
• Weigh accurately 0.5g of phenolphthalein indicator in a beaker.
• Dissolve the indicator in 50% aqueous ethanol with constant stirring.
• Transfer the solution to 100ml volumetric flak.
• Filter if precipitate is observed.
• Transfer the indicator to labeled indicator bottle.

9) Potassium chromate 5%

• Potassium chromate is used for the determination of chloride in sample.

• Weigh 5g of potassium chromate in a beaker.
• Dissolve it in distilled water. Transfer the solution to 100ml volumetric flak.
• Dilute to mark with distilled water.
• Transfer the solution to labeled indicator bottle.

10) Xylenol orange 0.1%

• The indicator is used for determination of dispersant in cooling water.

13
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: PREPARATION OF LABORATORY REAGENTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-WRK-04
ISO 14001 -
OHSAS 18001 - PAGE NO: 14 of 14
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

• Weigh accurately 0.1g of xylenol orange indicator in a beaker.

• Dissolve the indicator in water. Transfer the solution to 100ml volumetric flak.
• Dilute to mark with distilled water.
• Transfer the indicator to labeled indicator bottle.

14
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Loading and unloading, Storage & use of gas cylinder.
ISO 9001 - DOC.NO: TH-IMS-OHS-WRK-01
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 1

PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 00

APPROVED BY: HOD EFFECTIVE DATE: 25.03.2008

Loading, unloading, Storage use of gas cylinder.

Gas cylinder used in laboratory for analytical purpose.

• Confirm cylinders are handled with care.

• There shall not be impact on valves and body of cylinders.
• Colour code to be checked for appropriate gas.
• Segregate the cylinder as per the colour code.
• Check sufficient ventilation in storeroom and there is no obstruction.
• Chain guard to be confirmed after loading and unloading.
• Leak check for the cylinder before and after connection
• Beware that hydrogen gas has special regulator of reverse threading and
cylinder is completely red in colour.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Moisture in Ammonia and Amide sampling and analysis.
ISO 9001 - DOC.NO: TH-IMS-OHS-L-WRK-02
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 1

PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 00

APPROVED BY: HOD EFFECTIVE DATE: 25.03.2008

Moisture in Ammonia and Amide sampling and analysis

General Work instruction: Precaution to be taken during sampling,

• Use safety shoes, helmet, safety goggles and hand gloves.

• Use lean and dry sample bottles.
• Before sampling, locate safety shower nearby and check it is working.
• Stand in opposite direction of wind.
• Avoid skin contact with sample.
• In case of emergency while sampling wash the affected body part with
sample quantity of water.
• Report to Shift-In-Charge and First Aid for additional help.

During sampling of anhydrous ammonia and amide,

• Grease the stopcock of sample bottle / ampoule.

• Before sampling fill the sample bottle / ampoule with nitrogen.
• For amide in ampoule prepare the homogeneous mixture of dry ice and
acetone bath.
• For hand lining the dry ice use asbestos / PVC gloves.
• During sampling first close sample line valve.
• Close the inlet stopcock of the sample bottle.
• Ensured the stopcock of the outlet of the sample bottle remain open
• Close the both (Inlet and Outlet) stopcock of the sample ampoule.
• Immerse the sample ampoule in dry ice acetone bath immediately to
avoid pressurization of the sample ampoule
• After amide sampling , site should be washed with ample amount of water
• Avoid water contact with sample.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Sampling.
ISO 9001 - DOC.NO: TH-IMS-OHS-L-WRK-03
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 2

PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02

APPROVED BY: HOD EFFECTIVE DATE: 20.10.2013

General Work instruction: Precaution to be taken during sampling,

• Use safety shoes, helmet, safety goggles and hand gloves.

• Use lean and dry sample bottles.
• Before sampling, locate safety shower nearby and check it is working.
• Stand in opposite direction of wind.
• Avoid skin contact with sample.
• In case of emergency while sampling wash the affected body part with
sample quantity of water.
• Report to Shift-In-Charge and First Aid for additional help.
• For sample collections at height, use full body harness and accompany a
person.

1. Sampling from tanker

• Use clean and dry sample bottles.

• Use bottle carrying create
• Use helmet with belt.
• Use ladder for climbing on tanker.

2. Liquid air

• Use PVC gloves and helmet with face shield.

• Stand in opposite direction of wind.
• Keep the sample container away from body during sampling handling.

3. CO/CO2 gas sampling

• Use helmet with face shield.

• While sampling, accompany a person.
• Stand in opposite direction of wind.
• Keep the sample container away from body during sampling handling.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Sampling.
ISO 9001 - DOC.NO: TH-IMS-OHS-L-WRK-03
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 2

PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02

APPROVED BY: HOD EFFECTIVE DATE: 20.10.2013

4. Methylamines, DMF, DMAc and formic acid (process sample):

• Stand in opposite direction of wind.

• For methyl amine: open discharge valve first, flush the sample and change
the septum regula rly (Once in 15 days)
• After formic acid sampling site should be washed with ample amount of
water.

5. Reactor, stripper, GV and MEA solution

• Use clean and dry sample bottle.

• Stand in opposite direction of wind.
• Use PVC gloves and helmet with face shield.
• After sampling site should be washed with ample amount of water.

6. Precaution to be taken during chemical handling

• Use safety shoes, face shield/ safety goggles and hand gloves.
• Avoid skin contact with chemicals.
• Pour chemicals with the help of clamp stand.
• Take extra care while handling chemicals like sulphuric acid, nitric acid
etc.
• Locate safety shower nearby and check it is working.
• In case of emergency while handling of chemicals, wash the affected body
part with plenty of water.
• Report to lab-In-Charge and First Aid for additional help.
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SAMPLE POINTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPLPT
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

A) CENTRAL LAB

1. Ammonia Plant ( Amm-I & Amm- II )

• Liquid ammonia
• GV solution
• Boiler: - R.G. Boiler, Aux. Boiler, Loop Boiler, New Loop Boiler
• Steam condensate: – Dearator, S.C., Aux. steam, Loop steam, New loop steam,Turbine
condensate, Stripper condensate
• Process Gas: - PRO, HTI, HTO, MTO, LTO, ABI, METHO, S-200 IN, S-200 OUT, S-50
OUT, TO HWP, FROM HWP, TO ARGON, FROM ARGON, REBOILER , Purge
• HGRU: – H2 product, Mem – in, Mem – out, Purge,
• HGRU BED: – A- BED, B – BED, C – BED, D – BED, E – BED, F – BED, G – BED,
H – BED, I – BED, J – BED, K – BED, L – BED, M-BED,O-BED,P-BED,INLET TO P,
PRIMARY OUT
• Sulphur: – NG, RIL, HDS, ZNO-A, ZNO-B
• Dew point – Dryer, DR-2, DR-3, DR-4, COMMON

2. Urea plant (Unit – 11, 21, 31)

• CO2 : Before passivation, After passivation

• Urea prills : Urea prills of each plant & bagging plant, Neem coated urea prill
• Vent : PC108, PC165, PC133
• Waste water : P-18, V7, V8, V6, V2, P27
• Reactor/Stripper : Reactor, Stripper, ME2, ME3, V3, MV52
• Dew point

B) CHEMICAL GROUP LAB.

DMF SAMPLE POINTS:

• D-911 Reactor, liquid sample
• D-912 bottom First column bottom, liquid sample
• TC-102 First column top, liquid sample
• D-914 Stripper column top, liquid sample
• F-915 Catalyst tank, liquid sample
• F-921 A & B Batch tanks
• F-919 Off specification tank, liquid sample
• F-922 A & B Main storage tank, liquid sample
DMAC SAMPLE POINTS:
• R-003 Reactor, liquid sample
1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SAMPLE POINTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPLPT
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

• T-!2 liquid sample

• T-17 liquid sample
• HE-14 liquid sample
• HE-28 liquid sample
• T-003 Batch tank A & B
• T-101 Main storage tank A & B
MAP (old & new) SAMPLE POINTS
• V-102 vapor sample
• V-203 bottom DMA product, vapor sample
• V-203 top MMA product, vapor sample
• V-202 bottom Effluent, liquid sample
• V-202 top MMA, DMA mixture, vapor sample
• V-201 bottom MMA, DMA and Water mixture, liquid sample
• V-201 top TMA product, vapor sample
• V-200 bottom MMA,DMA,TMA and water mixture, liquid sample
• T-202 A & B TMA product batch tank, vapor sample
• T-203 A & B MMA product batch tank, vapor sample
• A&B DMA product batch tank, vapor sample

Formic acid.
• T 202 A/B Formic acid Batch Tank
• T 301 A/B Formic acid Storage
• T 103 Methyl formate Storage tank.
C) HEAVY WATER LAB.
• Plant Inlet Gas D/D+H
• 12 T1 Synthesis Gas Outlet D/D+H
• Main Cracker Gas outlet
• Purifier Liq. Amide
• 12T1 Liq. Amide
• 17 unit Amide
• 14C1 Potassium content
• 12V2 Potassium content
• 17C4 reflux. Potassium content
• 25V1 D2O purity
• 18V10 A/B/C D2O purity
• 25V4 D2O purity
• Reject From UGP ( New ) D2O purity
• Trapper outlet gas O2

2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: SAMPLE POINTS.
ISO 9001 - DOC.NO: TH-IMS-QCL-SPLPT
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 3
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 01
APPROVED BY: HOD EFFECTIVE DATE: 25.05.2012

D) WATER TREATMENT LAB.

WTP - I (Thermax)
• Anion A,B & C
• MB A,B & C
• DM Tank
• Degasser
• Cation A,B & C
WTP-II (BPMEL)
• Anion 1,2 & 3
• MB 1,2 &3
• PMB 1, 2 & 3
• DM Tank
• Degasser
• Cation 1,2 & 3

E) EFFLUENT TREATMENT LAB.

• Water samples :
• North drain.
• South drain.
• Gail,.
• pH Sea.
• pH irrigation.
• P 18 Urea condensate.
• P 34 EUST
• HWP,
• ACF inlet,.
• ACF outlet.
• Settler.
• Stripper condensate, .
• CF outlet.
• ETU Samples

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FREUENCY OF SAMPLING
ISO 9001 - DOC.NO: TH-IMS-QCL-FREQ
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 4
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.04.2013

FREQUENCY OF ANALYSIS.
• AMMONIA PLANT
SR.NO. NAME OF SAMPLE FREQUENCY
1. NATURAL GAS (APM), RELIANCE GAS FOR ONCE IN FIFTEEN DAY
TOTAL ANALYSIS & SULPHUR
2. PROCESS GAS PER LINE ONCE IN WEEK
3. HGRU ONCE IN FIFTEEN DAY
4. SULPHUR IN N.G., ZnO Outlet ONCE IN FIFTEEN DAY
5. LIQUID AMMONIA STORAGE TANK ONCE IN MONTH
6. PROCESS WATER, COOLING WATER, GV DAILY EXCEPT SUN,HOLIDAY
SOLUTION, STRIPPER & EFFLUENT
7. RAW MATERIAL AS PER REQUIREMENT
8. REBOILER AS PER REQUIREMENT
9. BAG & THREAD AS PER REQUIREMENT
10. OIL ANALYSIS, AS PER REQUIREMENT

• UREA PLANT ANALYSIS

SR.NO. NAME OF SAMPLE FREQUENCY
1. UREA PRILLS THRICE IN A DAY
P-18 THRICE IN A DAY
3. V6, V7, V8, P34, V2, P18 ONCE IN A DAY
4. REACTOR STRIPPER,ME2, ME3, V3, ONCE IN A WEEK EACH UNIT
ME52, PC108 (11,21,31) EACH
5. CO2 DAILY
6. P1 TWICE IN AWEEK EACH UNIT
7. COOING WATER ONCE IN A DAY
8. NEEM COATED UREA/ NEEM OIL AS PER REQUIREMENT

• WATER TREATMENT PLANT

SR.NO. NAME OF SAMPLE FREQUENCY
1. ANION , MB, DM TWICE IN A SHIFT
2. AMM COND, UREA COND. TWICE IN A SHIFT
3. P18 TANK, P18 LINE TWICE IN A SHIFT
4. STRIPPER COND. ONCE IN A DAY
5. STEAM COND. ONCE IN A DAY
6. BOILER TWICE IN A SHIFT
7. RAW WATER, COOLING WATER,SETTLER ONCE IN A DAY
8. MIDC TWICE IN A SHIFT

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FREUENCY OF SAMPLING
ISO 9001 - DOC.NO: TH-IMS-QCL-FREQ
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 4
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.04.2013

• DIMETHYLFORAMIDE PLANT

Sr.No. Sample point ( DMF plant) Frequency of sampling

1 D-911 Reactor, liquid sample Per shift
2 D-912 bottom First column bottom, liquid sample First shift
3 TC-102 First column top, liquid sample As per requirement
4 D-914 Stripper column top, liquid sample Per shift
5 F-915 Catalyst tank, liquid sample As per requirement
6 F-919Off specification tank, liquid sample As per requirement
7 F-915 Catalyst tank, liquid sample As per requirement
8 F-921 A & B Batch tanks As per requirement
9 F-921 A & B Batch tanks As per requirement
10 F-919 Off specification tank, liquid sample As per requirement
11 F-922 A & B Main storage tank, liquid sample As per requirement

• DIMETHYL ACETAMAINE PLANT

Sr.No. Sample point ( DMAC plant) Frequency of sampling
1 R-003 Reactor, liquid sample Per shift
2 T-!2 liquid sample As per requirement
3 T-17 liquid sample As per requirement
4 HE-14 liquid sample Per shift
5 HE-28 liquid sample As per requirement
6 T-003 Batch tank A & B As per requirement
7 T-101 Main storage tank A & B As per requirement
8 F-921 A & B Batch tanks As per requirement
9 F-921 A & B Batch tanks As per requirement
10 F-919 Off specification tank, liquid sample As per requirement
• MAP( old & new )

Sr.No. SAMPLE POINTS Frequency of

sampling
1 V-102 vapor sample As Per
requirement
2 V-203 bottom DMA product, vapor sample As Per
requirement
3 V-203 top MMA product, vapor sample As Per
requirement
4 V-202 bottom Effluent, liquid sample As Per
requirement
2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FREUENCY OF SAMPLING
ISO 9001 - DOC.NO: TH-IMS-QCL-FREQ
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 4
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.04.2013

5 V-202 top MMA, DMA mixture, vapor sample As Per

requirement
6 V-201 bottom MMA, DMA and Water mixture, liquid sample As Per
requirement
7 V-201 top TMA product, vapor sample As Per
requirement
8 V-200 bottom MMA,DMA,TMA and water mixture, liquid As Per
requirement
9 T-202 A & B TMA product batch tank, vapor sample As Per
requirement
10 T-203 A & B, MMA product batch tank, vapor sample As Per
requirement
11 T-204 A & B DMA product batch tank, As Per
requirement
• Formic acid

Sr.No. SAMPLE POINTS Frequency of

sampling
1 T 202 A/B Formic acid Batch Tank As Per
requirement
2 T 301 A/B Formic acid Storage As Per
requirement
3 T 103, Methyl formate Storage tank. As Per
requirement

• HEAVY WATER LAB.

Sr.No. Sample point Frequency of sampling
1 Synthesis Gas ( CO / CO2 content) As per requirement
2 Synthesis Gas ( Moisture content) As per requirement
3 Plant Inlet Gas ( Deuterium) Daily
4 12T1 Gas Outlet ( Deuterium) Daily
5 Cracked Gas outlet ( Deuterium) Daily
6 Purifier Liq. ( Amide ) As per requirement
7 12T1 Liq. (Amide ) As per requirement
8 25V1( Old) Daily
9 25V4( Old) Daily
10 18V10 A/B/C Daily
11 Reject From UGP ( New ) Daily
12 Deuterium Gas & liquid samples Once in three months.

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FREUENCY OF SAMPLING
ISO 9001 - DOC.NO: TH-IMS-QCL-FREQ
ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 4
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 02
APPROVED BY: HOD EFFECTIVE DATE: 01.04.2013

• EFFLUENT TREATMENT LAB.

• Water samples : Frequency of sampling – Daily
• North drain,
• South drain,
• Gail,
• pH Sea,
• pH irrigation,
• P 18 Urea condensate,
• P 34 EUST
• HWP,
• ACF inlet,
• ACF outlet,
• Settler,
• Stripper condensate,
• CF outlet,
• ETU Samples

4
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 1 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL/01-A

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 2 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-A Ist page

2
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 3 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-A 2nd page

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 4 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-B

4
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 5 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-C

5
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 6 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-D

6
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 7 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

7
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 8 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-02-B 1st page

8
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 9 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-02-B 2nd page

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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 10 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-E 1st page

10
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 11 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-E 2nd page

11
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 12 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CL-01-F

12
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 13 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS-FR-QCL-22-A

13
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 14 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-01-G

14
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 15 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-01-H

15
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 16 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

CHEMICAL GROUP LAB

TH-IMS/FR/QCL-CGL/01
Analysis report of Methanol
Date :
Report No: -
Date & Time :.
Ref. No.-

Tanker No. & Results

Tests
Specification Grade A/B/C

1) Appearance CLEAR & Free from suspended solids

Methanol content
Min 99.9 / Min 99.8 / Below 99.8
(% Wt.)
3) Color (APHA) < 15

4) Water(ppm) 1000 Max /2000 Max / >2000

5) Sp. Gravity at 20 °C 0.792 – 0.798

6) Acidity Index
0.02 %wt Max.

7) Permanganate Test 30 Minutes, Min.

8) Non – Volatile
0.001 % wt Max .
matter

Remarks: The sample passes as per grade A/B/C specifications.

Dy.Chief Chemist /Chief Chemist

To,
→S.I. ( DMF C.ROOM)
→O/C

16
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 17 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/03
CHEMICAL GROUP LABORATORY
Analysis report of Acetic Acid tankers.
Date :
Report No: -
Date & Time :.
Ref. No.-
Tanker No. & Results.

Tests Specifications Grade

A/B/C

CLEAR &FREE
FROM SUSPENDED
1) APPEARANCE
SOLIDS.

Min 99.8 /Min 99.7 /

2) ACETIC ACID ( % wt )
Below 99.7%
0.15 MAX / 0.15 MAX
3) FORMIC ACID (% wt )
/ Above 0.15%
0.03 MAX / 0.03 MAX
4) ACETALDEHYDE (% wt )
/ Above 0.03%
0.2 MAX / 0.3 MAX /
5) WATER ( % )
Above 0.3 %
6) COLOR (APHA) 15 MAX / 15 MAX /
Above 15
Remarks. The sample / samples is/are passing the test of grade A/B/C specifications.

Dy.Chief Chemist /Chief Chemist

To,
→Shift Incharge ( DMF )
→C.M.M. ( Stores )
→O/C

17
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 18 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

GENERAL SHIFT ANALYSIS: TH-IMS/ FR/QCL-CGL//05

Date.
Cooling Water Analysis
Process Water Analysis of CO Plant
MAPO CO/F. MAP R.G. Boiler Steam Pro. MEA
Tests Tests Aux.Boiler
LD A. NEW Boiler feed water Cond. cond Conc.%
pH pH
Conductivity Cond.
µmhos µmhos
Turbidity(NT
Silica(ppm)
U)
T.
Phosphate
.Hardness(pp
m)
Ca. Hardness
(ppm)
Mg. Hardness
Process Gas Analysis of CO Plant
(ppm)
M.
alkalinity(pp
H2 CO
m) Tests Reformer F-303
Product Product
Chloride
(ppm)
Solid content
Disparsant
CO2 % DMF plant %
.(ppm)
Vap
Phosphate
Ar+O2 % oris
.(ppm)
er
Iron.(ppm) N2 %
CH4 %
Free chlorine.
CO %
(ppm)
H2 %
DMF Storage / Drumming
pH of Acidity as HCOOH
Refra. Basicity
Color 20% Cond.of 20% Density at (ppm) Water %
Appearance Index at as DMA
APHA aqu. aqu. Soln. 200C Methanol / DMAC ( ppm) Purity
200C (ppm)
Soln. (ppm)

DMAC Storage / Drumming

pH of F.Acid storage
Cond.of Refra. Acetic
Color 20% Density at Water
Appearance 20% aqu. Index at acid % Purity purity
APHA aqu. 200C (ppm)
Soln. 200C (ppm)
Soln.

Effluent.
Cond.
Turbidity M-Alk.
PLANT pH Micro Dew point 0c
(NTU) (ppm)
mhos
MAP/DMF/DMAC sample result
COMMON point
CO/FORMIC Inst
COMMON Air.
18
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 19 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

S.I - DMF /CO-FOR./ O.M.(Chem.) / DGM (Chem.) /O/C Chief chemist.

TH-IMS/FR/QCL-CGL/06 A
METHYL AMINE PLANT (OLD – 31 UNIT ) OR ( NEW – 11 UNIT ) Date
First shift
Time Source NH3% MMA% DMA% TMA% MeOH% H2O% N/C

Second shift
Time Source NH3% MMA% DMA% TMA% MeOH% H2O% N/C

Third Shift
Time Source NH3% MMA% DMA% TMA% MeOH% H2O% N/C

FR/QCL-CGL/06 B
DMF PLANT ANALYSIS REGISTER
FIRST SHIFT Date
Time Source pH Cond Color DMA% MeOH(ppm) DMAC ( Water Misc. Remark
(µmhos) APHA ppm) ( ppm)

SECOND SHIFT
Time Source pH Cond Color DMA% MeOH(ppm) DMAC ( Water Misc. Remark
(µmhos) APHA ppm) ( ppm)

THIRD SHIFT
Time Source pH Cond Color DMA% MeOH(ppm) DMAC ( Water Misc. Remark
(µmhos) APHA ppm) ( ppm)

FR/QCL-CGL/06 B
DMAC PLANT ANALYSIS REGISTER
FIRST SHIFT Date
Time Source pH Cond Color DMA% Acetic acid % Water Misc. Remark
(µmhos) APHA ( ppm)

SECOND SHIFT
Time Source pH Cond Color DMA% Acetic acid % Water Misc. Remark
(µmhos) APHA ( ppm)

THIRD SHIFT
Time Source pH Cond Color DMA% Acetic acid % Water Misc. Remark
(µmhos) APHA ( ppm)

shift chemist

19
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 20 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/06 C

RASHTRIYA CHEMICALS & FERTILISERS LIMITED, THAL

raYT/Iya koimaklsa evaM fiT-laayaJasa- ilaimaToD

FORMIC ACID PLANT/fa^ima-k Aamla

LABORATORY ANALYSIS/ p`yaaogaXaalaa ivaXlaoXaNa

paarI I/
DATE /-idnaMak: : SHIFT - II/III

METHYL SO4
SAMPLE FORMIC
WATER FORMATE CAT. TDS PPM COLOUR Fe
TIME/ POINT/ CH3OH % ACID %
PPM / % % % % APHA/ PPM /
samaya sa^Mpla imaqa^naa^la fa^ima-k
paanaI imaqa^[la k^T^laIsT iT.DI.esa rMga Aayana-
p^a[NT Aamla Cl
fa^mao-T
PPM

chemist

20
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 21 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/07
RASHTRIYA CHEMICALS & FERTILIZERS LTD,
THAL UNIT, TAL- ALIBAG 402208 DIST-RAIGAD.MAHARASTRA STATE

CHEMICAL GROUP ABORATORY CERTIFICATE

FR/QCL-CGL/07

Anhydrous –MMA/DMA/TMA Date

Name of the product
Solution -
Tanker / Truck No
Reference No. Challon No.

To
M/s

RESULTS

NH3 MMA DMA TMA WATER

Appearance
% % % % %

Chemist /Chief Chemist

Chemical group lab.

21
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 22 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

RASHTRIYA CHEMICALS & FERTILIZERS LTD,

THAL UNIT, TAL- ALIBAG 402208 DIST-RAIGAD.MAHARASTRA STATE

CHEMICAL GROUP ABORATORY CERTIFICATE

TH-IMS/FR/QCL-CGL/08

Name of the product Di Methyl Formamide

Date
Bulk /Drum No.
Tanker / Truck No
Reference No. Challon No.

To.
M/s

RESULTS

Color in PH of 20 % aq. Cond. of 20 % aq. Density at 20 °C Refractive Index

Appearance
APHA Solution at R.T. Solution in µmhos Gms/cc at 25 °C

Basicity as Acidity as Dimethyl

Moisture in
DMA HCOOH Methanol in ppm Acetamide Purity in %
ppm
(ppm) (ppm) ( ppm)

Chemist /Chief Chemist

Chemical group lab.

22
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QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 23 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

RASHTRIYA CHEMICALS & FERTILIZERS LTD,

THAL UNIT, TAL- ALIBAG 402208 DIST-RAIGAD.MAHARASTRA STATE

CHEMICAL GROUP ABORATORY CERTIFICATE

TH-IMS/FR/QCL-CGL/09

LABORATORY- REPORT

Date
Name of the product Dimethyl Acetamide
Tanker / Truck No
Reference No. Challon No.

To,
M/s

RESULTS
Color in PH of 20 % aq. Cond. of 20 % aq. Density at 20 °C Refractive Index
Appearance
APHA Solution Solution in µmhos Gms/cc at 25 °C

Acidity as
Acetic acid Moisture in Purity in
(ppm) (ppm) %

Chemist /Chief Chemist

Chemical group lab.

23
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 24 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

RASHTRIYA CHEMICALS & FERTILIZERS LTD,

THAL UNIT, TAL- ALIBAG 402208 DIST-RAIGAD.MAHARASTRA STATE

ANALYTICAL REPORT OF FORMIC ACID

TH-IMS/FR/QCL-CGL/10
Date ;

Formic Acid
Bulk / Drum No.
Tanker / Truck No
Reference No. Challon No.

To
M/s

Appearance.;

Non Volatile
Purity Chloride Sulphate Matter
Tests Colour
% % %
%
Specs. < 50 85.0 Min. 0.003 max 0.003 max. 0.008 max.

Chemist /Chief Chemist

Chemical group lab.

24
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 25 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/11
Anhydrous Amines ( Unit )
Month

Date NH3 MMA DMA TMA CH3OH water

P
u
r
i
Graph area
t
y Date

I
m
p
u
r
i
t
y
Graph area

Chief Chemist

Chemical group lab.

Date

25
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 26 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/12
DMF Batch Tank
Month

CHEMICAL GROUP LAB

dmf Cond CH3OH DMAC H20
Date pH
% µmhos (ppm) (ppm) (ppm)
% DMF % PURITY FOR MONTH

P
u
r
I GraphDatearea
t
y
pH

C
O
N
D. Graph area
Date

H20, DMAC , METHANOL & H2O

GRAPH AREA
CH3OH
&
DMAC
Date .
Dy .C. Chemist
Chemical group lab
Approved by
Chief Chemist

ChiefChemist
Chemical group lab.

26
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 27 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/13
DMAC Batch Tank

DMAC Cond. A.acid h20

Date pH % DMAC PURITY FOR THE MONTH
% µmhos (ppm) (ppm)
P
u
r
I Date
t
y

P
H DMAC BATCH .TANK PH & COND.

&

C
O
Graph area
Date

N
D
W
A A. ACID
T GRAPH AREA
E
H2O
R
&
A
C Date
I
D

Approved by.

Dy. C. Chemist. Chief Chemist

Chemical group lab. Chemical Group lab.

27
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 28 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-CGL/14
Formic acid Batch Tank

sul
Purity % Formic acid PURITY FOR THE
Date pha chloride NVM)
% MONTH
te
P
u
r
I
t Date
y

P
H Formic acid BATCH .TANK sulphate
& chloride
&

C
O
Graph area
Date

N
D

Chief Chemist
Chemical Gr. Lab.

28
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 29 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Shift log book of HWP TH-IMS/FR/QCL-HWL/01 1st page

29
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 30 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

30
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 31 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Shift log book of HWP TH-IMS/FR/QCL-HWL/01 2nd page

31
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 32 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Shift log book of HWP TH-IMS/FR/QCL-HWL/01 3rd page

32
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 33 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Shift log book of HWP TH-IMS/ FR/QCL-HWL-01 4th page

33
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 34 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

FR/ QCL-HWL /02

34
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 35 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Water Treatment Laboratory TH-IMS/ FR/QCL-WTPL/01

SHIFT ANALYSIS REPORT : - ( I / II / III )

Plant Samples pH Conductivity in ppm Silica in ppm Turbidity NTU/any other

Anion A
Anion B
Anion C
WTP-I MB A
MB B
MB C
DM -I Thermax
Anion 1
Anion 2
Anion 3
WTP - II MB 1
MB 2
MB 3
PMB 1
PMB 2
PMB 3
DM - II BPMEL
Ammonia Condensate
Urea Condensate
V2/P18 Tank
V2 Tank
P18 Line

Chemist -

35
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 36 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Raw & Cooling water Report ( general shift report) TH-IMS/FR/QCL-WTPL/02

WATER TREATMENT PLANT LABORATORYANALYTICAL REPORT
DATE: TIME
: SAMPLE: BPMEL SETTLER OUTLET, R.C.F. RESERVOIR & S.G.P. COOLING WATER.
SOURCE: BPMEL (SET. OUTLET), R.C.F. RESERVOIR AND S.G.P. COOLING TOWER.
TEST BPMEL (SET. OUTLET)
RAW WATER COOLING WATER
PH
COND ( µmhos )
T. D. S.( ppm)
IRON - (ppm)
O.PHOS./T.PHOS ppm
R. SILICA ( ppm)
T. HARDNESS . ( ppm)
Ca.HARDNESS ( ppm)
M. ALKALINITY ( ppm)
P. ALKALINITY ( ppm)
SULPHATE ( ppm)
CHLORIDE ( ppm)
FREE CHLORINE ( ppm)
DISPERSANT ( ppm)
TURBIDITY (NTU)

MB & DM ANALYSIS CATION & DEGASSOR

TESTS THERMAX BPMEL TESTS THERMAX BPMEL
MB DM MB DM Cation Degassor Cation Degassor
R.SILICA F.M.A (.ppm)
In ppb CO2 (ppm)

CONDENSATE ANALYSIS CATIONIC & ANIONIC LOADS

Tests Ammo. Cond. Urea Cond. LOADS THERMAX BPMEL
PH
Conductivity µmhos CATIONIC
R. Silica in ppb ANIONIC

COPY TO :
1) Shift In charge (W.T.P.) / ( S.G.P.) Manager

36
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 37 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/03 Report of MIDC Water

WATER TREATMENT PLANT LABORATORYANALYTICAL REPORT
M.I.D.C.SAMPLES
Sr. Date TEST / prIxaNa SETTLER INLET SETTLER OUTLET FILTER OUTLET
No.
TURBIDITY / TribaDITI IN NTU
COND. ./ knDkTIvaITI µmhos
M. ALKALINITY/ema.AlklaInaITI(
ppm)
FREE CHLORINE/ÍI.@laaorIna
(ppm)
PH / pI eca

M.I.D.C.SAMPLES

Sr. Date TEST / prIxaNa SETTLER INLET SETTLER OUTLET FILTER OUTLET
No.
TURBIDITY / TribaDITI IN NTU
COND. ./ knDkTIvaITI µmhos
M. ALKALINITY/ema.AlklaInaITI(
ppm)
FREE CHLORINE/ÍI.@laaorIna
(ppm)
PH / pI eca
M.I.D.C.SAMPLES

Sr. Date TEST / prIxaNa SETTLER INLET SETTLER OUTLET FILTER OUTLET
No.
TURBIDITY / TribaDITI IN NTU
COND. ./ knDkTIvaITI µmhos
M. ALKALINITY/ema.AlklaInaITI(
ppm)
FREE CHLORINE/ÍI.@laaorIna
(ppm)
PH / pI eca
M.I.D.C.SAMPLES

Sr. Date TEST / prIxaNa SETTLER INLET SETTLER OUTLET FILTER OUTLET
No.
TURBIDITY / TribaDITI IN NTU
COND. ./ knDkTIvaITI µmhos
M. ALKALINITY/ema.AlklaInaITI(
ppm)
FREE CHLORINE/ÍI.@laaorIna
(ppm)
PH / pI eca

Chemist

37
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 38 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/04
WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/000/2000 Report Date :

1) Name of the chemical – Resins.
2) Date of Receipt :-
3) 3) No. of Samples:- )
4) Date of Analysis :-
5) In word No.:-
6) P.O. No. –
7) Batch No. :

ANALYSIS REPORT :-

Specifications Anion / Cation Anion Resin Cation Resin

Tests
Ionic form Chloride / Hydrogen
Effective Size 0.5 – 0.6 mm / 0.5 – 0.6 mm
Exchange Capacity 1.2 meq./ml & 2.0 meq./ml minimum.
Moisture Content 50 ±2 / 50 ±2 %
Settled Density 0.67-0.71 gms/ml & 0.80-0.84 gms/ml
Partical size
< 50 U.S.Mesh < 1.0 % / < 1.0 %
Screen Size 16 to 50 U.S. mesh ( WET)
Whole beads.
Cracks

Remark : -
Manager
(W. T. P. LAB)

Through Chief Manager

C.M.M. (Stores)

O.C.

38
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 39 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/05

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/000/2000 Report Date :

1) Name of the chemical – Silica Jel.
2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :-
5) Invoice No.:- .
6) P.O. No. –

ANALYSIS REPORT :-

Tests Party's Specifications. Laboratory Report.

Particle Shape
Particle Size (mm) 3 - 6 mm
Bulk Density gms / Lt. 0.835 gms / Lt
Water Adsorption Capacity (%) 25.0 %

Remark : -

Manager.
W.T.P.Laboratory

TO,

C.M.M.(Store)

39
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 40 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/ (REC/QCL-WTPL/05) Report Date :

7) Name of the chemical :– Activated Alumina.

8) Date of Receipt :-
9) No. of Samples :- )
10) Date of Analysis :-
11) Inward No. :-
12) P.O. No. :–
ANALYSIS REPORT :-

Tests Specifications. Laboratory Report.

Particle Shape Spherical Ball
Bulk Density gms / cc. 0.80 gms / cc
Moisture % 2.0 % max
Particle size ( 5.0 - 8.0 mm ) -
> 8.0 mm -
< 5.0 mm -
Water Adsorption Capacity (%) 20 % min

Manager
W.T.P.Laboratory.

C.M.M. (Stores)

C.M.. ( Lab.)

D.G.M. ( T / S )

D.G.M. ( Amm. plant )

O.C.

40
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 41 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/06

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/000/2000 Report Date :

1) Name of the chemical – Activated carbon.
2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :-
5) In word No.:-
6) P.O. No. –

ANALYSIS REPORT :-

TESTS PARTY SPECIFICATIONS LAB. REPORT REMARK

Appearance --
Moisture % 3.2 %
Apparent Density gms/cc 0.483 gms / cc
Iodine No. mg/g 1127 mg/g
Mesh Size 6 × 16
 6 Mesh 4.5 %
 < 16 Mesh 3.1 %
PH Value Alkaline

Chief Chemist
(W. T. P. LAB)
Through Chief Manager

C.M.M. (Stores)

O.C.

41
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 42 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/07

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/000/2000 Report Date :

Name of the chemical – Kem watreat Chemicals

1) Date of Receipt :-
2) No. of Samples:-
3) Date of Analysis :-
4) In word No.:-
5) P.O. No. –
ANALYSIS REPORT :-
Kem Watreat Type Batch N. Tests Remark
No
pH Sp.gr. State Ca-Value Zinc PO4
I

II
III
IV
V
VI
VII
Note: - 1) Sp.gr. = Specific gravity in gms/cc
2) Ca-Value = Calcium Sequestering Value in mg/ml
3) Zinc in %
4) PO4 in %
5) O.K. indicates result meets with given specifications.

Manager
(W. T. P. Lab.)
Through Chief Manager

C.M.M. (Stores)

O.C.

42
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 43 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No.: RM / WTPL/. (REC/QCL/WTPL/08) Report Date :.

1) Name of the chemical – MORPHOLENE

2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :- .
5) In word No.:- .
6) P.O. No. –

ANALYSIS REPORT :-
MORPHOLENE.

Specifications Lab results

1) Appearance : Colourless Liquid.

2) Purity % : 98.5 % Min

Remark : - Result matches with the given specification, Hence it is O.K.

Manager
(W. T. P. Lab)

C.M.M. (Stores)

C.M. ( T / S )

C.M. ( C.C.Lab )

O.C.

43
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 44 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No.: RM / WTPL/. (REC/QCL/WTPL/08) Report Date :.

1) Name of the chemical –

2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :- .
5) In word No.:- .
6) P.O. No. – 4300008351.

ANALYSIS REPORT :-
UCON - 50

Specifications Lab results

1) Appearance : Clear liquid.

2) Color : 200 APHA Max.

3) Moisture % : 0.15 % Min

4) PH of 10% solution : 5.5 to 7.5

5) Sp. Gravity : 1.057

Remark : - Result matches with the given specification, Hence it is O.K.

Manager
(W. T. P. Lab)

DGM. (ammonia)

C.M.M. (Stores)

C.M. ( T / S )

C.M. ( C.C.Lab )

O.C.

44
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 45 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No.: RM / WTPL/. (REC/QCL/WTPL/08) Report Date :.

1) Name of the chemical –

2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :- .
5) In word No.:- .
6) P.O. No. – 4300008351.

ANALYSIS REPORT :-
UCON - 50

Specifications Lab results

1) Appearance : Clear liquid.

2) Color : 200 APHA Max.

3) Moisture % : 0.15 % Min

4) PH of 10% solution : 5.5 to 7.5

5) Sp. Gravity : 1.057

Remark : - Result matches with the given specification, Hence it is O.K.

Manager
(W. T. P. Lab)

DGM. (ammonia)

C.M.M. (Stores)

C.M. ( T / S )

C.M. ( C.C.Lab )

O.C.

45
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 46 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-WTPL/09

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No. : RM/WTPL/000/200 Report Date

Name of the Chemical – Potassium Carbonate

test Specifications results
Total alkalinity as K2CO3 % by mass. Min. 98.0%
Loss on heating at 150 deg.C. % by mass Min. 2.0%
Chloride as KCL % by mass. Min. 0.015 % /0.10 %
Iron as Fe % by mass Min. 0.002% / 0.005%

Name of the Chemical – Hydrazine Hydrate

test Specifications results
Hydrazine hydrate % by mass. Min. 80.0%
Relative density at 20 deg.C. Min. 1.05gms/cc
pH of 1% solution. Min. 10.5

Name of the Chemical – Caustic soda lye.

test Specifications results
NaoH % by mass Min. not known, pro rata basis
Temp degC. Min. not known
Specific Gravity in gms/cc. Min. not known

Manager
(W. T. P. Lab.)

Through Chief Manager

C.M.M. (Stores)

46
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 47 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

WATER TREATMENT PLANT LABORATORY

ANALYTICAL REPORT

Ref. No.: RM / WTPL /. (REC/QCL-WTPL-09) Report Date :.

1) Name of the chemical – Glycine

2) Date of Receipt :-
3) No. of Samples:-
4) Date of Analysis :- .
5) In word No.:-
6) P.O. No. – .

ANALYSIS REPORT :-
GLYCINE.

Specifications Lab results

1) Appearance : White crystalline powder.

.
2) Purity % : 98.5 % Min

3) Sulphate % : 0.006 %.Max.

4) Chloride % : 0.007 % Max.

5) Loss on heat : 0.20 % Max

6) PH of 1% solution : 5.5 to 7.0

Remark : - Result matches with the given specification, Hence it is O.K.

Manager
(W. T. P. Lab)

C.M.M. (Stores)

DGM (Amm )

C.M. ( T / S )

C.M. ( C.C.Lab )

O.C.
47
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 48 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-ETPL/02

EFFLUENT TREATMENT LABORATORY

DATE INLET OUTLET SR2 M.L.S.S. Sign.

pH C.O.D. pH C.O.D. pH SR3A SR3

chemist

48
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 49 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-ETPL/03

EFFLUENT TREATMENT LABORATORY

Month
Date Day pH F.Amm T.A.N. T.K.N NO3. TSS OIL D.O. C.O.D. B.O. PO4-2 TEMP. Sign.
. N D.

chemist

49
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: FORMATS
ISO 9001 - DOC.NO: TH-IMS-QCL-FORM
ISO 14001 -
OHSAS 18001 - PAGE NO: 50 of 50
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

TH-IMS/FR/QCL-ETPL/01

EFFLUENT TREATMENT LABORATORY

Date Day Sample Point pH Ammonia Sign.

chemist

50
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: DOCUMENT OF EXTERNAL ORIGIN
ISO 9001 - DOC.NO: TH-IMS-QCL-EXTOR
ISO 14001 -
PAGE NO: 1 of 3
OHSAS 18001 -
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

DOCUMENTS OF EXTERNAL ORIGIN

Documents Location Responsibility

1 Haldor Topso manual (Ammonia)
Chief Manager
2 Snam Progetti manual, FCO Book (Addendum), Central lab.
(lab.)
1985 for urea.)
3 I.S. 7330-1988 for Resin and silica gel analysis
4 I.S. 7129-1993,
I.S. 12086-1987 WTP lab Sectional head
I.S. 248-1984
I.S. 4200-1984, for Other raw material
5 Indian std. Book for methanol
6 Indian std. Book for Acetic acid
Chemical
7 Indian std. Book for formic acid Gr. Lab. Sectional head
8 Acid Amines technologies for amines.
64/Con/02/06/1992
9 Haldor Topso manual for CO plant analysis
10 Annual Book of ASTM Stds. ( 1994 ), 11.01 and
11.02 ( For Water )
11 Vogel book of Practical organic Chemistry, Fifth
HWP lab Sectional head
Edition.
12 Heavy Water analysis manual by Alphonse and
HWP Board.
13 Chief Manager
GV solution analysis manual Central lab.
(lab.)

1
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: DOCUMENT OF EXTERNAL ORIGIN
ISO 9001 - DOC.NO: TH-IMS-QCL-EXTOR
ISO 14001 -
PAGE NO: 2 of 3
OHSAS 18001 -
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Documents Location Responsibility

Instrument Manual DM/QCL-CL/01 TO 11
1 Lab India UV Spectrophotometer software
2 Win-Chrome software
3 Euro Glass software
4 Euro Glass ( ECS 3000)
5 Euro glass manual EGM 1700
6 PHD6 Gas detector manual
7 pH Meter ( lab India)
Chief Manager
8 Conductivity meter ( lab. India) Central lab.
(lab.)
9 Perkin Elmer Gc manual
10 Perkin Elmer Gc software
11 Perkin Elmer GC Interface manual
12 Foss Operating manual
13 Brookfield Viscometer
14 Gas Chromatograph Chemito
15 AND Gr-200
16 AND HX-3000
Instrument Manual DM/QCL-HWL/01 TO 06
1 Mass Spectrometer
2 pH meter
3 Conductivity meter, HWP lab Sectional head
4 Flame Photo meter
5 Gas Chromatograph Chemito
6 Manual of Anton Paar DMA 58 /5000 density
meter
Instrument Manual DM/QCL-WTPL/01 TO 05

1 UV spectrophotometer ( 1700)
WTP lab Sectional head
2 pH Meter ( lab India)
Conductivity meter (lab. India)
3

Documents Location Responsibility

2
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: DOCUMENT OF EXTERNAL ORIGIN
ISO 9001 - DOC.NO: TH-IMS-QCL-EXTOR
ISO 14001 -
PAGE NO: 3 of 3
OHSAS 18001 -
PREPARED BY: SECTIONAL HEAD ISSUE NO: 01 REVISION NO: 03
APPROVED BY: HOD EFFECTIVE DATE: 10.05.2016

Instrument Manual DM/QCL-CGL/01 TO 19

1 Manual of Shimadzu Balance
2 Manual of Mettler Balance
3 Three star Conductivity meter
4 Three star pH meter
5 Manual of Turbidity meter
6 PICO Conductivity meter
7 PHAN pH meter
8 Manual of Refractometer
9 Manual of UV Spectrophotometer 160A Chemical
10 Gr. Lab. Sectional head
Manual of 701 KF Titrino
11 Manual of 702 SM Titrino
12 Manual of 787 KF Titrino
13 Manual of Anton Paar DMA4500 density meter
14 Manual of Shimadzu 14B GC
15 Manual of Mak-Analytica GC
16 Manual of 746 VA Trace Analyzer
17 Manual of Digital Burette
18
19

Instrument Manual DM/QCL-ETPL/01 TO 02

1 UV Spectrophotometer ( Chemito) ETP Lab Sectional head
2 BOD Instrument manual

3
 DEPARTMENTAL IMS MANUAL
QUALITY CONTROL LABORATORY
TITLE: Aspect Register
DOC.NO: TH-IMS-4-ASP-14
ISO 9001 -
ISO 14001 - 4.3.1 PAGE NO: 1 OF 1
OHSAS 18001 - ISSUE NO: 02 REVISION NO: 00
PREPARED BY: SECTIONAL HEAD EFFECTIVE DATE: 10.05.2016
APPROVED BY: HOD
Note - L Aspect- Legal compliance related aspect, L/HW Aspect- Legal hazardous waste management aspect, R Aspect- Resources conservation related aspect, E Aspect- Energy conservation related aspect
Environment Interested parties Legal
Plant/Department, Area, Resources Significance weightage Reference Document No.
Sr. No. Environmental Aspect Air Water Noise Land/soil Employees Surroundings Global Requir.
Activity S F S F S F S F S F S F S F S F Σ( X F))
Σ(S ΣS X ΣF
14. Laboratory Severity S = Serious 4, Moderate 3, Minor 2, Marginal 1.
Frequency F = continuous 4, Frequency>1 in month 3, Infrequent>1in a year 2, improbable 1. Yes - Y, No- N
14.1 Loading, trasportation, unloading of material
TH-IMS-QCL-EMP-01, 02, 10, 08. TH-IMS-OCP-02, TH-IMS-
14.1.1 Chemicals Spillage,leakage from the bottles 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 10 72 N REC/QCL/24
Exhaust release to atmosphere 1 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 10 72 N
14.1.2 Glassware Breakage of glasswares 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 2 11 81 N
14.1.3 H2, N2,Argon and LPG Leakage due to cylinder valve failure 2 1 1 1 2 1 1 1 1 1 1 1 1 1 2 1 12 88 N TH-EMS-EMP-121,TH-IMS-OCP-05,TH-IMS-QCL-SMP-03 /04
cylinder Exhaust release to atmosphere 1 2 1 1 1 1 1 1 1 1 2 1 1 1 1 1 11 81 N /06/08

14.1.4 Dry ice / liquid air Wastage due to continuous evaporation 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 1 10 72 N

14.2 Storage of material
14.2.1 Exhaust release to atmosphere 1 1 1 1 1 1 1 1 1 1 2 1 1 1 1 1 10 72 N TH-IMS-QCL-EMP-01, 02, 10, 08. TH-IMS-OCP-02, TH-IMS-
Chemicals REC/QCL/24
Spillage, leakage of the bottles 1 1 1 1 1 1 1 1 1 1 1 1 1 1 2 1 10 72 N
14.2.2 Cylinders Leakage due to cylinder valve failure 2 1 1 1 1 1 1 1 2 1 1 1 1 1 2 1 12 88 N
14.3 Use of chemicals and gases
14.3.1 H2, N2,Argon and LPG Leakage due to cylinder valve failure 2 1 1 1 2 1 1 1 1 1 1 1 1 1 2 1 12 88 N TH-EMS-EMP-121,TH-IMS-OCP-05,TH-IMS-QCL-SMP-03 /04
cylinder N /06/08
Burning of gas 2 1 1 1 1 1 1 1 2 1 1 1 1 1 2 1 12 88
Hydrogen generator Gas generation 1 1 1 1 1 1 1 1 2 1 1 1 1 1 2 1 11 80 N TH-IMS-OCP-03

14.3.2 Chemicals,Dry ice, liquid Spillage,leakage of the bottles 1 1 1 1 1 1 2 1 1 1 1 1 1 1 2 1 11 80 N TH-IMS-QCL-EMP-01, 02, 10, 08. TH-IMS-OCP-02, TH-IMS-
air REC/QCL/24
Use of chemicals 1 1 2 1 1 1 2 1 1 1 1 1 1 1 2 1 12 88 N
14.4 Sampling & Analysis
Raw material & Products Spillage of chemicals 1 1 2 1 1 1 1 1 2 1 1 1 1 1 1 1 11 80 N
( Urea,Neem coated Liquid/ solid waste genration 1 1 2 1 1 1 2 1 2 1 1 1 1 1 1 1 12 88 N
TH-EMS-6-OCP-76,TH-IMS-QCL-EMP-02, TH-IMS-
14.4.1 Urea,neem oil,Liquid QCL-WRK-02, TH-IMS-QCL-SMP-03,04,06,08
Ammonia,DMF,DMAc, N
Amines & FA) Vapour generation 2 1 1 1 1 1 1 1 2 1 1 1 1 1 1 1 11 80
Sample & carrier gas released to atmosphere 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 1 10 72 N TH-IMS-REC/QCL/24
14.4.2 Instrumental Analysis
Liquid effluent generation 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 1 10 72 N Th-IMS-QCL-SMP-05

HDPE / jute bag / Solid waste genration of cut bags & packing of
14.4.3 1 1 1 1 1 1 2 1 1 1 1 1 1 1 2 1 N TH-EMS-6-OCP-74
Thermocol & PVC material chemical bottles & instruments.
11 80
Benfield ( GV) /MEA
N TH-IMS-QCL-EMP-10
14.4.4 solution Spillage of solution 1 1 2 1 1 1 2 1 2 1 1 1 1 1 1 1 12 88
14.4.5 Breakage of glassware while adding H2O to amide 1 1 1 1 1 1 1 1 3 1 1 1 1 1 1 1 11 80 N TH-IMS-6-QCL--EMP-04
Ammonia /Amide
Catching fire during analysis & Vapour generation 1 1 1 1 1 1 1 1 2 1 1 1 1 1 1 1 10 72 N
14.4.6 Calibration of instruments
Gas effluent generation 2 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
10 72
N
TH-EMS-6-OCP-75,TH-IMS-REC/QCL/24
liquid effluent generation 1 1 2 1 1 1 1 1 1 1 1 1 1 1 1 1 10 72 N
14.5 Disposal
Sample disposal &
L/HW- AspectTH-EMS-6-OCP-74/TH-IMS-6-QCL--
washing of lab. Effluent generation 2 1 2 1 1 1 1 2 1 1 1 1 1 1 1 1 N
14.5.1 EMP-03
Glasswares. 12 90
empty chemical bottles liquid & gas effluent generation 2 1 2 1 1 1 1 2 1 1 1 1 1 1 1 1 12 90 N
14.6 Legal requirement
Weights and measurment
14.6 Y Weights and measurment act 1976 with PHP
act