GHATGE PATIL INDUSTRIES LIMITED
GUIDELINES ON CHEMICAL ANALYSIS
PROCESS – 07 – DESIGN & DEVELOPMENT
Document Number
Revision / Update
Date
GPIL-L03-P07-D&D-DI-A010-R03-22052019
03
22.05.2019
1.0
Purpose and scope:
To establish a method for determination of alloying & residual elements by spark atomic emission
vacuum spectrometry. This method is primarily intended to test alloy steel, stainless steel &
aluminum materials for compliance with chemical specifications (Refer Working Band Table 1).
2.0
Normative reference:

3.0
ASTM E415
Responsibility:
QA-QC engineer shall perform this test.
4.0
System :
o
Material composition shall be determined on a heat basis (or a re-melt ingot basis for re-melt
grade materials) in accordance with this manufacturer standard.
o
The chemical composition shall conform to the requirements of the
applicable material
specification
o
This method is applicable to alloy steels, stainless steels and aluminium. The working band
defined is as mentioned in table 01
o
The spectrometric determination of the chemical composition of metals is a comparative method.
The light intensities of actual measurement are compared with the intensities of known samples,
which were measured for the preparation of the calibration curves.
o
A capacitor discharge is produced between flat, ground surface of the disc specimen and conically
shaped electrode. The discharge is terminated at a predetermined intensity time integral of a
selected iron line, or at a predetermined time, and the relevant radiant energies of the analytical
lines are recorded (refer manufacturer’s instruction for detailed operation of machine).
o
The most sensitive lines of arsenic, boron, carbon, nitrogen, phosphorus, sulfur, and tin lie in the
vacuum ultraviolet region. The absorption of the radiation by air in this region is overcome by
evacuating the spectrometer or by use of a vacuum ultraviolet transparent gas and flushing gas
chamber with argon.
o
Excitation source shall be capable of providing electrical parameters required to spark the sample.
o
Spark chamber shall be automatically flushed with argon. The spark Chamber shall be mounted
directly on the spectrometer and shall be provided with a spark stand to hold a flat specimen and
lower counter electrode rod form. Follow manufacturer’s recommendation for cleaning the spark
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 1 of 7
chamber. During continuous operation, this typically should be done every 24 hours. Follow the
manufacturer’s recommendations for cleaning entrance lens or window.
o
During the first use of the spectrometer equipment an assortment of homogenous sample shall be
analyzed. Refer Table 2
o
Analyze results should correspond with a permissible tolerance to certified concentration values.
The assortment should be hold at stock and used for periodical spectrometer check. Refer Table
3
o
The equipment shall have a stable operation temperature. Refer manufacturer’s manual for
stabilizing instructions.
o
The system must be present in a properly recalibrated state.
Element
Steel & S.S.
Aluminium
C
0.003 - 2.50
-
Si
0.002 - 3.50
0.003 - 12.0
Mn
0.003 - 18.0
0.002 - 1.50
P
0.005 - 0.50
-
S
0.005 - 0.40
-
Cu
0.005 - 4.00
0.002 - 8.00
Al
0.002 - 1.50
Reference
Cr
0.003 - 30.0
0.002 - 0.50
Mo
0.005 - 7.00
-
Ni
0.003 - 30.0
0.002 - 4.00
V
0.003 - 5.00
0.001 - 2.00
Ti
0.002 - 2.00
0.001 - 0.50
Nb
0.003 - 1.50
-
Co
0.005 - 10.0
0.002 - 0.400
W
0.005 - 15.0
-
Pb
0.005 - 0.5
0.003 - 1.50
Fe
Reference
0.002 - 3.00
Zn
-
0.002 - 10.0
Sn
0.01 - 0.50
0.01 - 0.30
Mg
-
0.003 - 10.0
Table 1
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 2 of 7
Sr. No
Material
Standard No.
1
Low Alloy Steel
BCS / SS No. 406/1
2
Stainless Steel
BCS / SS CRMM 475
3
Aluminum
55 XGO2D5
Table 2
Grade
Low alloys steel
Stainless Steel
Aluminum
SS 406/1
SS 475
55 X G02 D5
Sample
No.
Element
%
tolerance
%
tolerance
%
tolerance
C
0.23
±0.010
0.05
±0.010
-
-
Si
0.31
±0.020
0.21
±0.020
10.03
±0.20
Mn
0.61
±0.020
0.89
±0.020
0.391
±0.020
S
0.049
±0.010
0.008
±0.005
-
-
P
0.009
±0.005
0.037
±0.005
-
-
Cr
2.1
±0.10
14.14
±0.50
0.76
±0.02
Mo
1
±0.10
1.59
±0.10
-
-
Ni
1.52
±0.10
5.66
±0.20
0.0652
±0.005
Co
0.006
±0.005
0.22
±0.050
0.0752
±0.005
Cu
0.28
±0.10
1.94
±0.10
0.406
±0.020
V
0.017
±0.005
-
-
0.0129
±0.005
Nb
-
-
0.22
±0.020
-
-
Mg
-
-
-
-
0.331
±0.020
Fe
-
-
-
-
0.557
±0.020
Zn
-
-
-
-
0.131
±0.010
Pb
-
-
-
-
0.067
±0.005
Sn
-
-
-
-
0.051
±0.005
Ti
-
-
-
-
0.018
±0.005
Table 3

Preparation of Specimens and Reference Materials
o
The specimens and reference materials shall be prepared in the same manner. A specimen cut
from a large sample section shall be of sufficient size and thickness for preparation and to properly
fit the spectrometer stand. A 10-mm to 38-mm thick specimen is normally most practical.
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 3 of 7
o
Ensure that the specimens are free from voids and pits in the region to be measured. Initially,
grind the surface with a 50-grit to 80-grit abrasive belt or disc (wet or dry) or mill the surface. If wet
grinding, perform the final grind with a dry abrasive belt or disc. A finer abrasive grinding media
(for example, 120-grit) may be used for the final grind, but is not essential. Specimen porosity is
undesirable because it leads to the improper “diffuse-type” rather than the desired “concentratedtype” discharge.
o
The specimen surface should be kept clean because the specimen is the electron emitter, and
electron emission is inhibited by oily, dirty surfaces.
o
Reference materials and specimens shall be refinished dry on an abrasive belt or disc before
being re-measured on the same area.
o
The specimen must have a sufficiently large prepared measured area. The area must be
representative of specimen. Known concentration variations at the surface must be removed (e.g.
De-carbonization of margin, marginal carbonization). The measuring point must fully cover the
hole of sparking chamber. In case of the sample is too small an adaptor shall be used. The point
must be free of grease and must be dry (free from water condensation in cold weather). The
sample surface shall never be moist.
o
For other sample preparation refer manufacturer’s instruction.

Preparation of Apparatus
o
Program the spectrometer to use the internal standard lines and one of the analytical lines for
each element depending on the mass fraction range and the individual spectrometer software.
o
Confirm argon supply is continuous & argon purifier is working before start of analysis.
o
Test the positioning of the spectrometer entrance slit to ensure that peak radiation is entering the
spectrometer chamber.
o
This shall be done initially and as often as necessary to maintain proper entrance slit alignment.
Follow the manufacturer’s recommended procedures. The laboratory will determine the frequency
of positioning the alignment based on instrument performance.

Electrical Parameters:
o
Burn parameters are normally established by the spectrometer manufacturer.
o
When parameter values are established, maintain them carefully. The variation of the power
supply voltage shall not exceed ±5 % and preferably should be held within ±2 %.
o
Burn and Measurement Conditions-A high-purity argon atmosphere is required at the analytical
gap. Molecular gas impurities, such as nitrogen, oxygen, hydrocarbons, or water vapor, either in
the gas system or from improperly prepared specimens, should be minimized.
o
Electrode System-The specimen, electrically negative, serves as one electrode. The opposite
electrode is a tungsten or silver rod, the tip of which has been machined to a 90° or 120° angled
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 4 of 7
cone. Use 3 mm, 4 mm, or 5 mm (60.1 mm) analytical gap. Condition a fresh counter electrode
with two burns to six burns using the operating conditions.

Preventive Maintenance shall be done as follows:
Parameter
Frequency
Servicing Of Spectrometer
Annually Twice
Spark Chamber Cleaning
Once in Two Weeks.
Argon Back Pipe Cleaning
Monthly once
Lens Polishing
During Servicing
Profiling
During Servicing
Vacuum
Pump
Inspection
Baking of Argon Purifier
Oil
Monthly once
Annually once

Standardization
o
Following the manufacturer’s recommendations, standardize on an initial setup or anytime that it is
known or suspected that readings have shifted. Make the necessary corrections either by
adjusting the controls on the readout or by applying arithmetic corrections.
o
Standardization shall be done anytime verification indicates that readings have gone out of
statistical control, refer table 3.
o
In the case of automatic corrections conducted by the spectrometer software, observe the
standardization factors and/or offsets. The factors and/or offsets are often presented in the
spectrometer software after standardization and/or stored in log files. Refer instrument manual or
instrument manufacturer for access to this information.

Verification
Verify that the instrument’s standardization is valid immediately after each standardization.

Calculation
Using the average results obtained, calculate the mass fractions of the elements from the analytical
curves.
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 5 of 7

Quality control requirements :
Sr.
No
Parameter
PSL 1
PSL 2
PSL 3/3G
PSL 4
Bodies, Bonnets,
1
End & Outlet
Connection
2
NA
Shall be performed on a heat basis & in accordance
with GPIL written specification.
Stems
Valve-bore
3
Shall be performed on a heat basis &
sealing
NA
NA
in accordance with GPIL written
mechanisms

specification.
Records requirements
Records of chemical composition shall be retained for a minimum of 10 years following the
date of manufacture.
Sr.
No
1
Parameter
PSL 1
PSL 2
PSL 3/3G
PSL 4
Bodies, Bonnets, End & Outlet
Connection ,Stems and Bore sealing
Material test records
mechanism
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Page 6 of 7
Reviewed by – for suitability & Approved by - For suitability &
Created – Prepared By
adequacy
adequacy
Name
Koli K D
Name
Barwade R A
Name
Sankpal V K
Position
Sr. Engineer
Position
AGM- QA&QC
Position
AVP- D&D
Date
22.05.2019
Date
22.05.2019
Date
22.05.2019
Signature
Signature
Signature
GPIL - ISO - API - IMS REFERENCES
LEVEL 02
LEVEL 03
ISO-API-IMS
ISO-API-IMS WORK
ISO-API-IMS FORMS -
PROCEDURES
INSTRUCTION
FORMATS - RECORDS
GPIL-L01-P05-MR-DI-
GPIL-L02-P07-D&D-
GPIL-L03-P07-D&D-DI-
GPIL-L04-P07-D&D-DI-
001
DI-007
LEVEL 01
ISO-API-IMS MANUAL
LEVEL 04
A010
A025
GPIL - ISO - API - IMS - STANDARD CLAUSE REFERENCES
ISO 9001: 2015
API SPEC Q1
ISO 14001: 2015
ISO 45001:2018
NA
NA
NA
NA
-
-
-
-
GPIL - ISO - API - IMS - Standard Clause References
API SPEC 6D
API SPEC 6A
Customer Requirement
NA
NA
NA
-
-
-
AMENDMENT HISTORY
Description of the Change / Amendment /
Rev No.
Date
01
14.10.2017
Originated
Process Owner
02
28.04.2018
Process Owner
03
22.05.2019
Revised document to include requirements of
ISO 45001:2018
Revised as per change in format
Revision
GPIL-L03-P07-D&D-DI-A010-R03-22052019
Approval Authority
Process Owner
Page 7 of 7