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INDEX

1.  SCOPE ...................................................................................................................................................... 2 

2.  REFERENCE DOCUMENTS .................................................................................................................... 2 
3.  APPLICABILITY ......................................................................................................................................... 2 
4.  SUPPLIER QUALIFICATION .................................................................................................................... 2 
5.  STARTING MATERIAL.............................................................................................................................. 2 
6.  GENERAL FORGING REQUIREMENTS.................................................................................................. 3 
7.  HEAT TREATMENT REQUIREMENTS .................................................................................................... 6 
8.  MECHANICAL TESTING........................................................................................................................... 7 
9.  CHEMICAL ANALYSIS.............................................................................................................................. 9 
10.  NDE & INSPECTIONS .......................................................................................................................... 9 
11.  TRACEABILITY ................................................................................................................................... 10 
12.  ALTERNATIVE FROM BAR ................................................................................................................ 10 
13.  PED REQUIREMENTS ....................................................................................................................... 11 
14.  HEAT TREATMENT QUALIFICATION PROCEDURE ....................................................................... 11 
15.  INSPECTIONS .................................................................................................................................... 13 
16.  CERTIFICATES ................................................................................................................................... 13 
17.  MATERIAL DATA SHEET ................................................................................................................... 14 

4 26/05/2015 Complete Rewriting – Includes Non-Shell Requirements P.Rossoni P.Rossoni

3 01/04/2015 Update new edition of SPE 77/302 +add F53 P.Rossoni P.Rossoni
2 01/02/2015 Change Company name – General update P.Rossoni P.Rossoni
1 20/10/2014 Firt revision D.Morelli P.Rossoni
Rev Date Description Issued Approved

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1. SCOPE 
Scope of this procedure is to define the Requirements for Metallic Materials used by the TIV for Manufacturing
of Valves in Accordance with API 6D Requirements

2. REFERENCE DOCUMENTS 
 ISO 9001:2008
 PED 97/23/EC
 NACE MR-01-75 / ISO 15156
 Applicable ASTM Standards (Latest Edition)
 API 6D 24th Edition
 Shell MESC 77/302 Ed. Feb 2015

3. APPLICABILITY 
This procedure is applicable to forged material purchased by the company for the manufacture of pressure
containing and pressure controlling parts:
- Body,
- Cover / Bonnets
- End Connections
- Ball
- Seats
- Stem
- Trunnion
- Welding Neck flanges
- Blind Flanges
- Drain / Vent Plugs

4. SUPPLIER QUALIFICATION 
On top of specific supplier qualification requirements, specified for each materials, all supplier must be qualified
by TIV according requirements settled by procedure CP 04 –“Supplier selection”

5. STARTING MATERIAL 
5.1. APPROVAL OF STARTING MATERIALS SUPPLIERS 
Only melt source facilities that are approved by the forging supplier shall be used to supply starting material
such as billet or ingot material.
The forging supplier shall have a documented procedure, fully implemented, for qualifying starting material
suppliers for each specific size and grade of starting material. The approval process shall be based on both a
quality assurance and a technical evaluation. The approval process shall establish the methodology by which
the starting material supplier will be evaluated on an ongoing basis to maintain their status as an approved
supplier.

The maintenance of an acceptable quality program, such as an ISO registration, is not sufficient
by itself to satisfy the above requirements.
Documented evidence that a starting material supplier has a historical and ongoing technical capability of
producing materials meeting this standard and who has proven, implemented procedures and capabilities in
place to consistently produce acceptable product is a minimum requirement. Options for the technical approval
of a starting material supplier include one or more of the following.

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- Supplier experience over an extended period of time. Demonstration of acceptable experience shall include
tests/inspections, quantity of material received, non-conformance analysis, etc.
- On-site technical audit at scheduled intervals. A new supplier shall be subject to an onsite technical audit, w

The forging supplier is responsible for ensuring that a starting material supplier has
implemented controls addressing the following for each size and grade of starting material ordered:
— chemistry controls;
— hydrogen controls;
— melting practice controls;
— teeming practice and ingot mold controls;
— hot work practice controls (method of forging, amount of reduction, forging temperature, etc.);
— cooling rate and method controls;
— ingot/billet cropping controls;
— starting material inspection and acceptance criteria (cleanliness requirements, limitations on
porosity or inclusions, grain size, secondary phases, microstructure, macrostructure, etc.) as applicable;
— material contamination controls (e.g. mercury, radioactivity).

5.2. STARTING MATERIAL SPECIFICATIONS  
Starting material requirements shall be documented in the form of material specifications by the forging
supplier.
Material specifications shall be developed by the forging supplier or the purchaser.
Material specifications shall include as a minimum:
— material grade, including element chemistry ranges;
— melting practices and ladle refinements;
— acceptable forging reduction range, if applicable;
— acceptable cleanliness level range,
— acceptable inspection practices and criteria.

The forging supplier shall document acceptance of incoming starting material to the requirements of the
material specification prior to use for production of forgings.

6. GENERAL FORGING REQUIREMENTS 
6.1. GENERAL  
All Forged materials shall be formed using a hot-working practice and heat treatment that produces a forged
structure throughout the material
The following are general requirement from TIV for production of forgings.
Deviations or alternatives be accepted, if supplier procedure is provided to TIV and accepted.

6.2. Manufacturing Procedure Specification  
The forging supplier shall prepare a manufacturing procedure specification to include, as a minimum, the
material specification and the general variables below:
- size of starting material, cut weight and tolerances;  
- evaluation process used for incoming material and for determining cropped length of starting material;  
- hydrogen flake‐control method (bake‐out, slow cool, etc.), if applicable;  
- hot‐working temperature range;  
- overall hot work ratio from starting material;  
- description of each forging operation, including general product configuration at the beginning and end of 
each different type of hot work or forging operation and hot‐work ratio for each step;  
- acceptable forging equipment for production;  
- inspection requirements;  
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- NDE, if applicable.  
- heat treat parameters (see clause 6)

As part of the Procedure, the forging steps shall be shown detailing initial and final dimensions during forging
for each step of the forging process. This will also include documentation of the heat or reheat temperature
ranges required for each hot work reduction step in a drawing and written documents.

6.3. FURNACE CALIBRATION 
Forging furnaces shall be calibrated in accordance with the forging suppliers written procedures.

6.4. FURNACE LOADING 
Each furnace load should consist of only one type of material and never of different materials of the same
shape and size. The material should firstly be placed at the bench at the entrance of the furnace.
To avoid mix-ups of materials, a chart will be compiled with the following information: the batch date, the
furnace identification number, and the plan of how the pieces are arranged within the furnace with relating heat
numbers

6.5. POSITIONING OF PIECES FOR FORGING WITHIN THE FURNACE 
Material is arranged within the furnace in such a way as not to burn or cast the pieces directly under the flame.
The pieces need to be sufficiently rotated as to facilitate a uniform heating.
- Pieces weighing over 150kg must be placed deep within the furnace without coming into direct contact
with the flame.
- Pieces weighing less than 150kg must be placed at the entrance of the furnace.

6.6. EXTRACTION OF PIECES FROM THE FURNACE 
The extraction of pieces from the furnace is done exclusively by means of a mechanical manipulator.
Each furnace is equipped with a digital thermometer with probe and picking stick to keep the temperature
under control
Thermocouples must be calibrated at least once per years and record of the last 5 years must be available for
review

6.7. HEATING AND HOLDING TIME 
The length of time pieces need to be left in the furnace to reach a uniform temperature is calculated at an hour
per inch. The attached table determines furnace temperature for pieces. An optical system (pyrometer) is used
to control furnace temperature.
Furnace tables, heating time parameters, and the pyrometer must be available for review.

6.8. FORGING 
Forging of pieces will be carried out with a minimum total ratio of approximately 3:1, based on the shape of the
piece to be forged, using the various free moulds and fixed moulds suitable for realisation of the piece
corresponding to the forge design.
If bars or forged blooms are used as starting materials, these must have a minimum forge ratio of 4:1.

the following are typical schematisations for the various forge operations for typical shapes

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6.8.1. Forging of  round pieces  or Discs 

6.8.2. Forging of Rings  

Once the piece is forged, the heat number must be marked with chalk or other suitable method and it will be
placed in the appropriate cooling area
Forged material should be stored in the appropriate cooling area. Once cooled, the heat number will be
rewritten in permanent ink.
Materials in austenitic steel are cooled in the appropriate vats / thanks, which are changed or each different
material in production

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7. HEAT TREATMENT REQUIREMENTS 
7.1. HEAT TREATMENT PARAMETERS 
The following are heat treat parameters, as applicable:
— furnace loading diagram, orientation and spacing of production parts;
— heat treat times and temperatures for each processing cycle;
— forging configuration and dimensions at time of heat treatment;
— quenching medium and type of agitation (water/polymer, forced, horizontal; or vertical quench, ID/OD, etc.);
— quench medium start and finish temperature and transfer time to quench.

7.2. FURNACES 
Heat treatments must be carried out using gas furnaces.
All heat treatment for mechanical properties shall be performed using furnaces calibrated in accordance with
paragraph 14 of this specification (API 6D 24th edition Annex F)
Furnaces shall be calibrated and surveyed at least annually.
The thermocouples and recorders are calibrated at least every 12 months and record shall be maintained for a
period not less than 5 years.
.
7.3. HEAT TREATMENT PROCEDURE 
Each heat treatment batch shall include:
- Forgings of different shapes but of similar thickness.
- Forgings of different types of steel but with similar treatment temperatures.

The forgings are loaded in the furnace in such a way as to guarantee an even treatment and an even cooling of
the whole load.
The heating and cooling rates are established according to the weight of the treatment load and the applicable
material specification
Unless indicated otherwise, treatment temperatures are defined by applicable material specification
A pyrometer can be used to verify that the temperature indicated by the furnace tools and the temperatures of
the pieces correspond.

Unless otherwise specified by material specification, Holding time is calculated as follows:

1 hour for every 25mm of thickness (considering the highest thickness of the pieces, or the thicker pieces if
different shape loaded).

7.4. QUENCHING OR SOLUTION HEAT∙ TREATMENT 
Water quenching and solution heat - treatments are carried out in the suitable vats
which have the following features:
• Adequate dimension for the pieces to be treated
• Maximum bath temperature: 60°C
• Water circulation in the vats guaranteed by 3 equidistant drainpipes with 0100
• Water cooling guaranteed by a cooling tower with complete circulation of the vat in 3 hours and a exit
temperature of 20°C

Waiting time from opening the furnace to immersion of the piece inwater can vary from
10 to 30 seconds according to weight.
Bath temperature is checked during the cooling process, using rod thermocouples

7.5. DOCUMENTATION 
Heat treatment Temperatures for each batch must be recorded,
when requested, heat treatment chart must be provided.to TIV,and shall be in any case available for review

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7.6. STATISTICAL PROCESS CONTROL 
All heat treatment procedures shall be subject to a statistical process control to ensure that the final material
properties comply with the applicable material standard.
In order to avoid over-application of inspection and testing per batch, particularly for smaller batches, pro-active
application of statistical process control of parameters which are critical to the manufacturer to produce goods
to the intended quality level is deemed a strong enabler to achieve product quality.

8. MECHANICAL TESTING 
8.1. TENSILE TEST REQUIREMENTS 
Tensile test specimens shall be removed from a fest test Coupon (TC) after the final heat treatment cycle.
Perform tensile tests at room temperature in accordance with the procedure specified in ASTM A370

Perform a minimum of one tensile test. All yield strengths shall be determined using 0.2 % offset method. –
‘The result of tensile test shall satisfy the applicable material specification requirements
If the results of the tensile test(s) do not satisfy the applicable requirements, two additional tests on two
additional test specimens (removed from the same TC with no additional heat treatment) may be performed in
an effort to qualify the material. The results of each of these tests shall satisfy the applicable requirements.

8.2. IMPACT TESTING 
Impact testing is required where this is a requirement of the applicable standard specification or design code
and whenever it is required for compliance to PED 97/23/EC Requirements.
Moreover all material suitable for a design temperature below -29°C shall be impact tested (except austenitic
grades)

The test method shall be V-notch technique in accordance with ASTM A 370
Where sub-size specimens are permitted or necessary, the required absorbed energy shall be adjusted
accordingly by the ratio of the specimen width parallel to the notch to the width of a full-size specimen (10mm)
as indicated in ASTM A370.

A minimum of one impact test, comprising a set of three specimens, shall be performed on a representative
test bar of each heat of the material in the final heat-treated condition.

Test specimens shall be cut from a separate or attached block taken from the same heat, reduced by forging
where applicable, and heat-treated to the same heat treatment, including stress-relieving, as the product
materials, except that it is not necessary to retest pressure-containing parts stress-relieved at or below a
previous stress-relieving or tempering temperature.
Impact test specimens shall be located at mid thickness.

The impact test shall be performed at the lowest temperature as defined by the applicable material
specification, or as defined by TIV requirements

If not otherwise stated in each specific material, Minimum Acceptance criteria are the following

Minimum Material Tensile Single specimen

Average
Strength NON PED PED
≤689 27J 21J 27J
>689 34J 26J 27J

Additional requirements for quality control purposes are provided for each specific material.

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8.3. HARDNESS TEST 
When required hardness test must be performed In accordance with ASTM E110;

8.4. TEST SAMPLE LOCATION 
Location for test samples is specified below, in case of forged round pieces or discs:

Test sample for forged round pieces (Longitudinal + transversal – when required by MDS)
On prolongation or on sacrificial piece

Location for test samples is specified below, in case of forged rings

Test sample for forged rings (Longitudinal + transversal – when required by MDS)
On prolongation or on sacrificial piece

NOTE: each test sample in above sketch represent a set of 1 Tensile specimen + 3 Charpy impact specimen

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9. CHEMICAL ANALYSIS 
9.1. CARBON EQUIVALENT 
The carbon equivalent (CE) shall be calculated with the following formula:

9.2. PREN NUMBER 
The PREN (Pitting Resistance Equivalent) shall be calculated as given in Equation:

PREN = wCr + 3.3(wMo + 0.5wW) + 16Wn

where
- wCr is the mass fraction of chromium in the alloy, expressed as a percentage mass fraction of the total
composition;
- wMo is the mass fraction of molybdenum in the alloy, expressed as a percentage mass fraction of the
total composition;
- wW is the mass fraction of tungsten in the alloy, expressed as a percentage mass fraction of the total
composition;
- wN is the mass fraction of nitrogen in the alloy, expressed as a percentage mass fraction of the total
composition.
- .
Per lot, one product analysis shall be made. One lot is defined as a group of valves manufactured for one heat
of material and heat treatment batch.

10. NDE & INSPECTIONS 
10.1. Visual Inspection 
Visual inspection of the production forging shall be performed in accordance with the forging supplier’s
procedures for cracks, laps, seams and other anomalies.
Results shall be documented and the material shall be dispositioned.
Any discontinuities discovered shall be evaluated and the disposition documented.

10.2. Nondestructive Examination (NDE) 
Production forgings shall be capable of meeting the NDE requirements requested by TIV specification.
NDE shall be performed as specified in the purchasing documents.

10.3. Dimensional inspection 
Dimensional inspection shall be performed on forgings produced
Each forging shall be inspected. The dimension indicated in TIV PO must be measured.
If not otherwise stated the general acceptance criteria is max -0 / +15mm with respect to the measures
indicated on the purchase order
Acceptance criteria for dimensions shall be as required by the purchaser’s written specification.

10.4. Repair By Welding 
Repair Welding Repair welding is not permitted on forgings produced to this specification.

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11. TRACEABILITY  
Full traceability of forgings shall be maintained with respect to material heat, with revision level and heat
treatment loads.
Forging qualification records shall be traceable to the Manufacturing procedure
Forgings shall be traceable to the applicable forging qualification record.

12. ALTERNATIVE FROM BAR 
Alternative from Bar is acceptable only when communicated to TIV prior to order.
When SHELL MESC 77/302 is applicable, Use of Bar for body and closures are in any case limited to Valves
4” (DN 100) and below .
Bar shall be supplied with material certificates in accordance with EN 10204 type 3.1, demonstrating that the
mechanical properties in all three main directions exceed the requirements of the material standard
specification:

Test sample position for bar (Tensile + Impact Test)

Following additional applies (when specified):

- ASTM A961 Supplementary requirement S50.1 shall be used to demonstrate that bar is delivered with
wrought microstructure;
- ASTM E381 and ASTM E340 test methods shall be used as applicable;
- The test sample shall be cut parallel to the longitudinal axis of the bar, at a location approximately one
diameter away from the end of the bar.

12.1. SUPPLEMENTARY TESTS FOR BAR STOCK 
Supplementary tensile and impact test shall be performed in addition to the mechanical property tests
prescribed in the material standard specification, as follows;
Number of tests and the test method shall be the same as prescribed in the material standard specification

Test locations and orientation:

The additional test specimen shall be removed from one representative bar selected from each heat and heat-
treatment load in the longitudinal, transverse and tangential orientation as close to the surface as practical;
NOTE: to avoid unfavourable mechanical test results, test samples need not be taken from the core region of
the bar that will be bored out to produce the valve.
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Where impact testing is a requirement of the applicable material standard specification the notch of the impact
test specimen shall be perpendicular to the nearest cylindrical bar surface (longitudinal and tangential
specimen) or perpendicular to the longitudinal axis of the bar (transverse specimen)
The acceptance criteria shall be in accordance with the material standard specification and this specification

13. PED REQUIREMENTS 
When components are addressed to PED Valves, the requirement of this specification must be integrated with
a Particular Material Appraisal (PMA) approved by 3rd party and provided by TIV in order stage.
Manufacturer of materials for PED application must have an appropriate quality-assurance system, certified
by a competent body established within the Community and having undergone a specific assessment for
materials. Quality Assurance system certificate of the Material manufacturer, must be provided by the supplier.

14. HEAT TREATMENT QUALIFICATION PROCEDURE 
14.1. INTRODUCTION 
This paragraph refer to annex F of API 6D 24th Edition
The below qualification procedure is a mandatory requirement. Alternative procedure, exceeding those
requirements may be proposed by forging manufacturer, and must be approved by TIV prior to use

All heat treatment of parts and TCs shall be performed with equipment meeting the requirements of this annex

14.2. Temperature Tolerance 
The temperature at any point in the working zone shall not vary by more than ±25 of (±13 0c) from the furnace
set-point temperature after the furnace working zone has been brought up to temperature.
Furnaces that are used for tempering, aging, andlor stress relieving shall not vary by more than ±15 of (±8 °C)
from the furnace set-point temperature after the furnace working zone has been brought up to temperature.

14.3. Furnace Calibration 
14.3.1. General 
The following provided details on the types of furnaces to be surveyed.

14.3.2. Temperature Survey Method for Calibration of Batch‐type Furnaces 
A temperature survey within the furnace working zone(s) shall be performed on each furnace at the maximum
and minimum temperatures for which each furnace is to be used.
A minimum of nine thermocouple test locations shall be used for all furnaces having a working zone greater
than 10 ft3 (0.3 m3).
For each 125 ft3 (3.5 m3) of furnace working zone surveyed, at least one thermocouple test location shall be
used, up to a maximum of 40 thermocouples. See Figure F.1 and Figure F.2 for examples of thermocouple
locations.

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For furnaces having a working zone less than 10 ft3 (0.3 m3), the temperature survey may be made with a
minimum of three thermocouples located either at the front, center, and rear or at the top, center, and bottom of
the furnace working zone.
After insertion of the temperature-sensing devices, readings shall be taken at least once every 3 min to
determine when the temperature of the furnace working zone approaches the bottom of the temperature range
being surveyed.
Once the furnace temperature has reached the set-point temperature, the temperature of all test locations shall
be recorded at 2-min intervals, maximum, for at least 10 min. Then readings shall be taken at 5-min intervals,
maximum, for sufficient time (at least 30 min) to determine the recurrent temperature pattern of the furnace
working zone.
Before the furnace set-point temperature is reached, none of the temperature readings shall exceed the set-
point temperature by more than ±25 ' F (±13 ·C).
After the furnace control set-point temperature is reached, no temperature reading shall vary beyond the limits
specified. The temperatures within each furnace shall be surveyed within one year prior to use of the furnace
for heat treatment.

14.3.3. Temperature Survey Method for Recalibration of Batch‐type Furnaces 
When a furnace is repaired or rebuilt, a new temperature survey shall be carried out before the furnace is used
for heat treatment, subject to the following.

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Repairs that return the furnace to the condition it was in at the time of the last furnace survey and calibration or
repairs that do not affect the temperature tolerance of the furnace shall not require a new temperature survey
and calibration

The SAE AMS 2750 sections on furnace modifications and furnace repairs shall be used to determine whether
a new furnace survey is required. All furnace repairs and modifications shall be documented and the
responsible Quality Assurance organization shall make determination whether an additional furnace survey and
calibration is required based on the repairs or modifications in accordance with AMS 2750.

F.3.4 Continuous-type Furnaces Method

Furnaces used for continuous heat treatment shall be calibrated in accordance with procedures specified in
SAE AMS-H-6875.

14.4.  Instruments 
14.4.1. General 
Automatic controlling and recording instruments shall be used.
Thermocouples shall be located in the furnace working zone(s) and protected from furnace atmospheres by
means of suitable protective devices.

14.4.2. Accuracy 
The controlling and recording instruments used for the heat-treatment processes shall be accurate to ±1 % of
their full-scale range.

14.4.3. Calibration 
Temperature-controlling and temperature-recording instruments shall be calibrated at least once every three
months.
Equipment used to calibrate the production equipment shall be accurate to ±0.25 % of full-scale range.

15. INSPECTIONS 
The supplier accepts to be visited in any moment of status and development of supply, without any notice, by
TIV personnel, either for the acceptance of control system, for the verification of manufacturing, or
preservations status of materials subject to purchase order.
In case of visits by customer, end user, third party, etc., the supplier should be noticed with necessary notice,
and should be available to receive the personnel charged by inspection.

16. CERTIFICATES 
If not otherwise stated on Purchasing order, the certification required should be in accordance with EN 10204,
type 3.1 .

NOTE: Certificate 3.1 issued by re-seller are not accepted. In case the material is provided by a re-seller, it
must be supplied the original certificate of the manufacturer.

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Any additional certification requirements should be specified in purchase order.
All certificates should be clearly stated, issued also in English language, and should indicate, on top of what
stated by the respective material standard, as follows:
• TIV purchase order
• Description of goods
• Complete material designation
• Declaration of Origin of raw materials
• Supply status
• Temperatures and times for heat treatments, for each batch
• Number of heat/identification/batch, which is stamped on the piece
• Complete chemical analysis
• Results of mechanical tests
• Results of harness tests

17. MATERIAL DATA SHEET 
Here attached the Material Data Sheet which includes the requirements for specific material Grade
Requirements of PED must be respected, whenever PED applicability mentioned in TIV purchasing information
(PO and attached specification)
Requirements of MESC 77/302 must be respected whenever MESC 77/302 applicability mentioned in TIV
purchasing information (PO and attached specification)
 

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