Materials and Qualification Procedures for Ships · Material and Qualification Procedures for Ships Book K ... Adequate quantity of catalyst ... procedure to verify that no significant

Materials and Qualification Procedures for Ships

Book K

Procedure 14-1

Approval of Gel Coat and Laminating Resins

Revision 1, December 2013

Material and Qualification Procedures for Ships Book K Procedure 14-1

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Lloyd’s Register Group Limited, its subsidiaries and affiliates and their respective officers, employees or agents are, individually and collectively, referred to in this clause as ‘Lloyd’s Register’. Lloyd’s Register assumes no responsibility and shall not be liable to any person for any loss, damage or expense caused by reliance on the information or advice in this document or howsoever provided, unless that person has signed a contract with the relevant Lloyd’s Register entity for the provision of this information or advice and in that case any responsibility or liability is exclusively on the terms and conditions set out in that contract.

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Approval of Gel Coat and Laminating Resins 1 Introduction

1.1 Application for approval

1.1.1 In order that consideration may be given to approval of a resin, the local Surveyors are to submit a report to Materials and NDE Department, giving the information listed in Sections 2 and 3 together with the results of approval tests carried out under their survey.

1.1.2 Data Forms GCR (Gel Coat Resins) and LRP (Laminating Resins for use in reinforced

Plastics) are to be used in the report (see Appendix A and B).

1.2 Scope

1.2.1 All gel coat and laminating resins employed in constructions moulded under LR survey are to be approved for this purpose prior to use. (LR does not accept orthophthalic gel coat resins).

1.2.2 In the case of gel coat resins, cosmetic aspects of pigmentation are excluded from any approval.

1.2.3 Where the resin is tested after elevated temperature cure or post cure conditions not in accordance with those specified by LR the approval will be valid only for these conditions.

1.3 Validity of approval

1.3.1 Initial approval, where granted, will be for a period of five years. Thereafter, approval may be extended for successive periods of five years, following re-testing and the submission of satisfactory test data.

1.3.2 The approval will be limited to a nominated site of manufacture. Where the product is manufactured at other sites, these are to be approved separately.


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1.4 Withdrawal of approval

1.4.1 Approval is given on the assumption that production material, when examined, will exhibit similar test results to those submitted, allowing for normal batch to

batch variation.

1.4.2 Approval is contingent on the adherence to the stated specification. Approval will be withdrawn if:

(a) The properties of the resin are found to deviate significantly from those on which the approval was originally granted.

(b) The resin proves to be intractable in use.

(c) The quality control procedures are not adhered to consistently.

(d) The manufacturer makes changes to the formulation, product name or reference number without notifying LR.

2 Information required for approval

2.1 Product details

2.1.1 The manufacturer is to provide the following product related details:

(a) Physical properties. The following information from the manufacturer's own data is to be recorded as appropriate in Part 1 of the relevant Data Form (see Appendix A and B):

(i) Specific gravity of the resin (liquid and cast)

(ii) Mineral content.

(iii) Acid value of styrenated resin.

(iv) Epoxide value.

(v) Volatile content.

(vi) Volume shrinkage on cure.

(vii) Viscosity.

(viii) Shelf life at room temperature.


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(ix) Geltime and catalyst details.

(b) Product literature. Manufacturer's current trade literature referring to the resin.

(c) Quality control. The manufacturer is to operate established quality control procedures capable of detecting any variations from the properties submitted for approval. A brief description of the quality control methods and frequency of testing is to be submitted.

2.1.2 Variants. Approval of a resin may be extended to its variants, such as thixotropic, pre- accelerated, sprayable, tropical, etc. Where approval is requested, full details of the associated quality controls are to be submitted to Materials and NDE Department. Where the formulation of a variant differs significantly from the original tested material, full tests will be required.

3 Approval test programme

3.1 General

3.1.1 Approval will be granted following a satisfactory examination of data from the tests detailed in Section 4. For laminating resins, additional tests are required as detailed in Section 5.

3.2 Testing

3.2.1

The tests are to be carried out by one of the following:

(a) LR’s own Materials Laboratory.

(b) An independent test house that has been accredited, by a nationally recognised body, for the tests undertaken with testing witnessed by an LR Surveyor.

(c) The manufacturer’s own test facility with testing witnessed by an LR Surveyor.

3.2.2

The test facility is to be staffed and equipped such that they are able to conduct the required tests in a competent manner.


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3.2.3 A copy of the test report, inclusive of all load/extension curves, is to accompany the application for approval and the completed Data Form

3.2.4

When testing is to be undertaken by LR’s own Materials Laboratory the following should be submitted to the Laboratory:

(a) 5 kg (5 litres) of the resin (preferably the non-thixotropic version).

(b) Adequate quantity of accelerator (if the accelerator to be used is not a cobalt solution). (c) Adequate quantity of catalyst (if the catalyst to be used is not Butanox M50).

(d) The correct mixing ratios by weight percentage.

(e) Parts 1 and 3 of the relevant Data Forms, Part 3 to be signed by the Quality Manager of the site of manufacture.

4 Approval tests

4.1 Test samples and specimens

4.1.1 For both gel coat and laminating resins, cast samples are to be prepared and cured under conditions identical to those of the intended use.

4.1.2 Where the resin is intended for use under ambient conditions, specimens are to be cured for 24 hours at room temperature (18°C to 21°C) followed by a postcure of 16 hours at 40°C.

4.1.3 If the resin is intended for use under elevated temperature curing conditions, specimens are to be cured at these temperatures.

4.1.4 The specimens are to be tested, using ISO standard methods, as given in Section 6, and the following test data reported in Part 2 of the relevant Data Form:

(a) Water absorption (seven days value). (b) Barcol hardness

(c) Flexural strength and modulus (not required for laminating resins) (d) Tensile strength at maximum stress and secant modulus.

(e) Elongation at break and at maximum stress.

(f) Temperature of deflection under load (not required for gel coat resins) .


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4.1.5 The minimum requirements for properties of cast gel coat and laminating resin are shown in Section 8.

5 Laminating resin: Additional tests on chopped strand mat (CSM) laminate

5.1 Test samples and specimens

5.1.1 The laminating resin under test is to be used to produce a laminate containing a nominal 1800 g/m2 of chopped strand mat reinforcement approved by LR and of 25-35 per cent glass content.

5.1.2 The test laminate is to be prepared using the curing conditions described in 4.1.2 and 4.1.3.

5.1.3 The laminate is to be tested, using ISO standard methods, as given in Section 6, and the following test data reported in Part 2L of Data Form LRP:

(a) Flexural strength, flexural rigidity modulus, tensile strength, secant modulus at 0,25 per cent and 0,5 percent strain in the dry condition.

(b) Flexural strength, tensile secant modulus at 0,25 per cent and 0,5 per cent strain after immersion in distilled water for 28 days at 35±2°C, followed by cooling to room temperature whilst still immersed in water.

(c) Compressive strength.

(d) Compressive modulus.

(e) Glass content by weight of laminate.

(f) Water absorption at room temperature after seven days immersion.

5.1.4 Minimum requirements for properties of chopped strand mat laminate are shown in Section 8.

5.1.5 Where an epoxide resin is to be tested, a compatible LR approved balanced woven roving, at a glass content of 50 per cent, is to be used in place of the chopped strand mat and tested in one principal fibre direction only.


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6 Standard test methods for approval of a resin

6.1 Introduction

6.1.1 The following information is provided for the guidance of manufacturers and the Independent Test Houses through whom data is established and submitted to LR, where approval is sought of a resin for constructions under LR's survey.

6.1.2 Tests conducted other than to ISO Standards below, or employing test specimens or testing conditions, (test speeds), differing from those stated will not be accepted unless the prior written agreement of LR has been given.

6.1.3 Tests conducted other than to ISO Standards below, or employing test specimens or testing conditions, (test speeds), differing from those stated will not be accepted unless the prior written agreement of LR has been given.

6.2 Cure/post-cure condition (ambient equivalent)

6.2.1 A cure/post-cure condition (ambient equivalent) is applicable in all cases whether a gel coat resin or laminating resin is under evaluation.

6.2.2 The cast resin/laminate is to be cured initially for 24 hours at room temperature (18°- 21°C) followed by a post-cure of 16 hours at 40°C.

6.2.3 Test results based on materials which have been subjected to more intensive cure conditions will not be approved by LR, unless intended for use at elevated temperatures.

6.3 Test methods

6.3.1 Gel coat resins (tests on castings): Table 14-1.6.1 gives details of the ISO test methods and speed of test.

6.3.2 Laminating resins (tests on CSM Laminate): Table 14-1.6.2 gives details of the ISO test method and speed of test.


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7 Additional test requirements for approval of air inhibited and `low styrene emission' or `environmental' resins

7.1 Introduction

7.1.1 Where resins which have been modified by the addition of waxes or polymers to provide `low styrene emission or air inhibited' materials are employed in the construction of reinforced plastics craft under the LR survey, LR requires that the use of such resins will not result in poor interlaminar adhesion if interruptions to the laminating process occur.

7.1.2 These types of resins are to be tested in accordance with the following test procedure to verify that no significant loss in interlaminar adhesion occur.

7.2 Test procedure

7.2.1 A test laminate based on four plies of 450 g/m2 chopped strand mat and of 25-35 per cent glass content is to be prepared in two stages (see 7.2.2). A conventional room temperature curing catalyst/accelerator system is to be employed for laminate preparation.

7.2.2 A laminate of two plies of 450 g/m2 chopped strand mat of 25-35 per cent glass content is to be prepared at a laboratory temperature of 18°-21°C and allowed to stand for four days at this temperature. After four days, a further two plies of mat are to be laminated onto the exposed surface and, after an initial cure at room temperature (18°-21°C) for 24 hours is to be post-cured at 40°C for 16 hours.

7.2.3 After cooling, the apparent interlaminar shear strength of the laminate is to be determined in accordance with ISO 14130, (conditioning of the test specimens may be omitted).

7.2.4 If the tests are undertaken at the resin manufacturer’s own laboratory the individual test values are to be reported accompanied by the broken test specimens

7.3 Alternative test procedures

7.3.1 By prior agreement, LR will accept alternative test procedures which are considered effective to demonstrate acceptable interlaminar adhesion behaviour.


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8 Minimum values for properties of gel coat and laminating resins

8.1 Minimum requirements - Gel coat resins

8.1.1 The minimum requirements for the properties of cast gel coat resins when tested according to the appropriate LR procedure are shown in Table 14-1.8.1.

8.2 Minimum requirements – Laminating resins

8.2.1 The minimum requirements for the properties of laminating resins when tested according to the appropriate LR procedure are shown in Tables 14-1.8.2 to 14-1.8.4.


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Table 14-1.6.1 Tests on unreinforced cast thermoset resin specimens

T e s t S t a n d a r d Tensile properties

Flexural properties

Water absorption

Temperature of deflection under load

ISO 527-2 ISO 178

ISO 62

ISO 75

Test speed = 5 mm/min Specimen 1A or 1B

T h i c k n e s s Test speed = mm/min

2 Method 1

Method A

NOTES 1. ISO 62 – where resins are intended for use under ambient conditions to avoid

additional post-curing, the requirement in ISO 62 for pre-drying the test specimen at 50C is to be omitted. The test result is to be expressed as mg of water absorbed.

2. ISO 527-2 – tensile properties are to be measured using extensometry.

Table 14-1.6.2 Tests on laminate specimens

Test Standard Tensile properties

Flexural properties

Compressive

properties

Interlaminar shear

Water absorption

ISO 527-4 ISO 14125

ISO 604

ISO 14130

ISO 62

ISO 1172

Test speed = 2 mm/min Specimens Types 2 or 3

Thickness

Test speed = mm/min 2

Test speed = 1 mm/min

Method 1 (See Note 1)

NOTES 1. ISO 62 – where resins are intended for use under ambient conditions to avoid

additional post-curing, the requirements in ISO 62 for pre-drying the test specimen at 50C is to be omitted. The test result is to be expressed as mg of water absorbed.

2. ISO 527-4 – tensile properties are to be measured using extensometry. 3. Tensile modulus values are to be determined using an extensometer which may

be removed for strain to failure.


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Table 14-1.8.1 Minimum requirements - Cast gel coat resins

Water absorption 70 mg maximum

Elongation at maximum stress 2,5% minimum Tensile

strength at maximum stress 40 N/mm2 minimum Flexural

strength 70 N/mm2 minimum

Barcol hardness As specified for full cure

Table 14-1.8.2 Minimum requirements - Cast laminating resin


Elongation at maximum stress 2% minimum

Tensile strength at maximum stress 40 N/mm2 minimum

Barcol hardness As specified for full cure

Temperature of deflection under load 55°C minimum Table 14-1.8.3 Minimum requirements - Chopped strand mat laminate

Tensile strength 200Gc + 30 (N/mm2)

Tensile secant modulus 15G c + 2,4 (kN/mm2)

Flexural strength 502Gc2 + 114,6 (N/mm2)

Flexural modulus 33,4Gc2 + 2,7 (kN/mm2)

Compressive strength 150Gc + 72 (N/mm2)

Compressive modulus 40Gc – 6 (kN/mm2)


NOTE Gc is the actual glass fraction of the laminate by weight


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Table 14-1.8.4 Minimum requirements - Woven roving laminate

Tensile strength 400Gc - 10 (N/mm2)

Tensile secant modulus 30G c + 0,5 (kN/mm2)

Flexural strength 502Gc2 + 106,8 (N/mm2)

Flexural modulus 33,4Gc2 + 2,2 (kN/mm2)

Compressive strength 150Gc + 72 (N/mm2)

Compressive modulus 40Gc – 6 (kN/mm2)


NOTE Gc is the actual glass fraction of the laminate by weight

��

MQPS 14-1 APPENDIX A GEL-COAT RESIN DATA FORM GCR

Word 97 version

Mat reference number or grade: Manufacturer: Address:

Resin Type: (see Note 1) Variants: (see Note 2)

Part 1-RESIN PROPERTIES Data from manufacturer’s own records (where applicable)

PROPERTY

Nominal Value

Tolerance

Test Method

S.G. of liquid resin:

S.G. of cured resin:

Acid value of styrenated resin: (mgKOH/g)

Epoxide value:

Total mineral content : (%)

Volatile content: (%)

Volume shrinkage on cure: (%)

Packaging details: Storage life at room temperature: Recommended storage temperature:

For cold cure systems

Catalyst/curing agent mix ratio: Geltime details:

Note 1: Please state whether isophthalic, neopentyl glycol, sprayable, pre-

accelerated, thixotropic, etc.

Note 2: State reference number and nature of modification

��MQPS 14-1 APPENDIX A

GEL-COAT RESIN DATA FORM GCR

Part 2- CAST RESIN TEST PROPERTIES

Tests to be conducted on specimens prepared using a conventional cold curing system, cured for not less than 24 hours at room temperature (18°- 21°C) and postcured for 16 hours at 40°C , or under agreed alternative curing conditions.

One copy of the Test House report and load extension curves must accompany this data summary form.

CAST RESIN PREPARATION

Catalyst or curing agent:

Quantity:

Accelerator type:

Quantity:

Initial cure temperature and time:

Post- cure temperature and time:



CAST RESIN TEST DATA

Property Unit Individual Test Values

Mean Property

Value

Test Method Used

Hardness

Barcol 934-1 meter

Flexural strength

N/mm2

Flexural modulus

kN/mm2

Tensile strength

N/mm2

Tensile secant modulus at 0.25% strain at 0.5% strain

kN/mm2

Elongation at break

%

Elongation at maximum Stress

%

Water absorption at 7 days

mg



Part 3 QUALITY CONTROL SCHEDULE

List below the tests carried out on the resin (alkyd, styrenated alkyd or finished product) for routine Quality Control purposes and the frequency of these tests.

Test

Frequency

Signature …………………………………. (on behalf of manufacturer)

Position

Date

ABCD APPENDIX B MQPS 14-1

LAMINATING RESIN DATA FORM LRP

Mat reference number or grade:

Manufacturer:

Address:

Resin Type: (see Note 1) Variants: (see Note 2)

Part 1-RESIN PROPERTIES Data from manufacturer’s own records (where applicable)

PROPERTY

Nominal Value

Tolerance

Test Method

S.G. of liquid resin:

S.G. of cured resin:

Acid value of styrenated resin: (mgKOH/g)

Epoxide value:

Total mineral content : (%)

Volatile content: (%)

Volume shrinkage on cure: (%)

Viscosity (poise)

Packaging details: Storage life at room temperature: Recommended storage temperature:

For cold cure systems

Catalyst/curing agent mix ratio: Geltime details:

Note 1: Please state whether isophthalic, orthophthalic, sprayable, pre-

accelerated, thixotropic, etc.



Part 2- CURED RESIN TEST PROPERTIES

Tests to be conducted on specimens prepared using a conventional cold curing system, cured for not less than 24 hours at room temperature (18°- 21°C) and postcured for 16 hours at 40°C , or under agreed alternative curing conditions.

One copy of the Test House report and load extension curves must accompany this data summary form.

CAST RESIN PREPARATION

Catalyst or curing agent:

Quantity:

Accelerator type:

Quantity:

Initial cure temperature and time:

Post- cure temperature and time:



CAST RESIN TEST DATA

Property Unit Individual Test Values

Mean Property

Value

Test Method Used

Hardness

Barcol 934-1 meter

Tensile strength

N/mm2

Tensile secant modulus at 0.25% strain at 0.5% strain

kN/mm2

Elongation at break

%

Elongation at maximum Stress

%


mg

Temperature of deflection under load

°C



Part 2L Tests on Chopped Strand Mat Laminated at 25-35% w/w Glass Content or Woven Roving at 50% Glass Content

Details of test laminate construction

Reinforcement manufacturer:

Grade:

Weight per ply:

Number of plies:

Catalyst type and concentration:

Accelerator type and concentration: (when required)

Actual weight used in laminate Reinforcement Resin preparation

Property Unit Dry Value *Wet

Value Test Method

Used (see section 6.3)

Flexural strength

N/mm2

Flexural modulus

kN/mm2

Tensile strength

N/mm2

Tensile secant modulus (dry) at 0.25% strain at 0.5% strain

kN/mm2

Compressive strength

N/mm2

Not Required

Compressive modulus

kN/mm2

Not Required

Glass content of test laminate

%


mg



Part 3 QUALITY CONTROL SCHEDULE

List below the tests carried out on the resin (alkyd, styrenated alkyd or finished product) for routine Quality Control purposes and the frequency of these tests.

Test

Frequency

Signature …………………………………. (on behalf of manufacturer)

Position

Date

Documents

Materials and Qualification Procedures for Ships · Material and Qualification Procedures for Ships Book K ... Adequate quantity of catalyst ... procedure to verify that no significant