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FOR BIS USE ONLY DOC:CHD 20 (1936)CDecember 2012

BUREAU OF INDIAN STANDARDS

Draft Indian Standard

INTUMESCENT FIRE RETARDANT PAINT(Water based)

(Not to be reproduced without the permission of BIS or used as STANDARD)

Last date for receipt of comments is 3103 2013

0 FORWARD(Formal clauses will be added later on)

1. SCOPE

1.1 This specification relates to intumescent fire retardant paint used in internal areas ofdifferent structures requiring fire protection. This paint, when exposed to fire, forms a cellularcarbonaceous char, 70 80 times thicker to its original thickness which provides heat insulationand also acts as an oxygen barrier thus preventing ignition of combustible substrate materials.The coating also helps in maintaining mechanical integrity of light alloy metallic structures, inview of its heat insulation property.

1.2 The paint shall be suitable for application by brush or by airless spray (with 5-7% de-ionised water) to provide uniform coating having thickness of 250 25 microns in single coat.Intumescent fire retardant paint is a water based single pack system and should be mixedthoroughly before use. A two coat system is recommended for protection of wood /plywood,electrical cables, aluminium and other polymeric materials. This paint can be applied directly

over wood / plywood substrates and on electrical cables after surface preparation. However,metallic substrates require suitable primers before application of intumescent paint.

2. REFERENCES

The standards listed in Annex A contain provisions which through reference in this text,constitute provisions of and necessary adjuncts to this standard. At the time of publication, theeditions indicated were valid. All standards are subject to revision and parties to agreementsbased on this standard are encouraged to investigate the possibility of applying the most recenteditions of the standards indicated in Annex A.

3. REQUIREMENTS

3.1 Composition

Intumescent fire retardant paint comprises of vinyl acetate acrylic co-polymer emulsion,intumescence agents and pigments. Ammonium polyphosphate, pentaerythritol, dicyndiamideare used as intumescence agents and titanium dioxide as pigment, where as vinyl acetate acrylicco-polymer is used as a binder. Phosphorus content in the pigment, when examined inaccordance with the method described in Appendix C shall not be less than 20%.

3.2 Keeping Quality

Intumescent fire retardant paint when stored in original container under normal conditions shall

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retain the properties described in this specification for a minimum period of twelve monthsfrom the date of manufacture.

3.3 The paint shall also conform to requirements given in Table 1.

Table 1: Requirement Of Intumescent Fire Retardant Paint(Clause 3.4)

Method of testSl.No.

(1)

Characteristics

(2)

Requirements

(3) Ref. to IS: 101 Annex

1 Color White/Off-White Part 4/Sec 2)

2 Preliminary examination Stirring should easily produce asmooth uniform paint suitablefor application by brush orairless spray (with 5-7% de-ionised water).

Part 1/Sec 2

3 Application properties

and finish

Paint film shall be uniform and

free from defects

Part 1 /Sec 4

4 Consistency Thixotropic Part 1/Sec 2

5 Drying time , minutes(At 65% RH), max.(a) Surface dry(b) Hard dry

60120

(Part 3 / Sec 1 )

6 Dry film thickness,microns

250 25 (Part3 / Sec 2)

7 Scratch hardness, gm,minimum(1000 g)

To pass the test Cl 3 of (Part 5/Sec 2)

8 Flexibility and

adhesion(Bend test)(using 25 mm diametermandrel)

To pass the test Cl 2 of (Part 5/Sec 2)

9 Mass / 10 litres, kg 13.70.3 (Part 1/ Sec 7 )

10 Percent pigment,Minimum

40 B

11 Percent volatile matter,Maximum

30 (Part 2 / Sec 2 )

12 Fire test(a) Char height, mm

Min

(b) Flame spreadLength, mm, maxc) Time after glow,Secd)Time after flaming,Sec

30.0

127

Nil

Nil

C

13 Keeping properties Not less than one year from dateof manufacturing

(Part 6/Sec 2)

NOTE - Theoretical covering capacity of intumescent fire retardant paint is approximately 2.0 sq. m / ltr onwooden surface and 2.5 sq. m / ltr on metallic surfaces at DFT 250 microns.

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4. PACKING AND MARK ING

4.1 Packing

The materials shall be packed in high density polyethylene / polypropylene container of 4 or 20ltr capacity. Container shall be fitted with a tight lid using gasket.

4.2 Marking

Each drum shall be legibly marked as under:

(a) Nomenclature of the stores indicating name of the paint.(b) Manufacturer name and his recognised trade mark, if any.(c) Net and gross weight of drums.e) Batch number or Lot number in code or otherwise;f) Month and year of manufacture; andg) A cautionary note as below

- Keep out of reach of children.- Dried film of this paint may be harmful if eaten or chewed.- This product may be harmful if swallowed or inhaled.

4.3 BIS Certification Marking4.3.1 The container may also be marked with the Standard Mark.

4.3.1.1 The use of the Standard Mark is governed by the provisions of Bureau of IndianStandards Act, 1986 and the Rules and Regulations made there under. The details of conditionsunder which the Iicence for the use of the Standard Mark may be granted to manufacturers orproducers maybe obtained from the Bureau of Indian Standards.

5 TEST METHODS

5.1Test shall be conducted as prescribed in various parts of IS 101 and various Annexes to thisstandard. References to the relevant clauses of these standards are given inCol 4 & 5of Table 1,and in 3.1 to 3.2.

5.2Quality of Reagents

Unless specified otherwise pure chemicals anddistilled water (see 1S 1070) shall be employedin tests.

NOTE Pure chemicals shall mean chemicals that do not contain impurities which affect the results of analysis.

A N N E X A(Clause 2)

LIST OF REFERRED INDIAN STANDARDS

IS No. Title

IS 101 Methods of sampling and test for paints, varnishes and related products(Part 1/ Part 1 Test on liquid paints (general and physical),

Sec 1) : 1986 Sec 1 Sampling (third revision)Sec 2) : 1987 Sec 2 Preliminary examination and preparation of samples for testing (Third

revision)Sec 4) : 1987 Sec 4 brushing test (third revision)Sec 7) : 1987 Sec 7 Mass per 10 litres (third revision)

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(Part 2/ Part 2 Test on liquid paints(chemical examination)Sec 2):1986 Sec 2 Volatile matter(third revision)

(Part 3/ Part 3 Test on paint film formation,Sec 1) : 1986 Sec 1 Drying time (third revision)Sec 2) : 1989 Sec 2 Film Thickness (third revision)

(Part 5/ Part 5 Mechanical tests on paint filmsSec 2) : 1988 Sec 2 Flexibility and adhesion tests (third revision)

IS 517:2004 Specification for methanol(Methyl alcohol) (second revision)IS 1070 : 1992 Reagent grade Water (third revision)IS 1303 : 1983 Glossary of terms relating to paint (second revision)

A N N E X B(Table 1, Sl. No.10)

DETERMINATION OF PIGMENT CONTENT

B-1 OUTLINE OF METHOD

This method describes the sampling and test for determination of pigment and non-volatilematter content in water based paints.

B-2 APPARATUS

B-2.1Centrifuge tubes, 50 ml, heavy-walled

B-2.2 Water bath

B-2.3 Drying Oven, capable of being maintained at 1052C

B-2.4 Analytical balance, Least Count 0.1mg.

B-2.5 Centrifugal machine, capable to swirl at minimum 3000 rpm.

B-3 REAGENTSB-3.1 Methyl alcohol, (IS 517).

B-3.2 Distilled water

B-3.3 Extraction Mixture -Mix 1 part of distilled water, 4 parts of methanol. Thisextraction mixture ensure maximum retention of pigment but does not fully extract resin.

B-4 PROCEDURE

B-4.1Weigh accurately 15 to 20 gm of well mixed material into a weighed centrifuge tube. Add40 to 50 ml of appropriate extraction mixture (see B-3.3) and mix thoroughly with the extractionmixture in the centrifuge tube. Whirl the tube at a minimum speed of 4500 rev/min until

maximum separation is effected. Decant the liquid and repeat the process thrice or more, ifrequired.

B-4.2 Place the tube containing the pigment on the water bath for half an hour for the solventsto escape. Keep it in an oven at 105 2C and weigh after drying to constant mass.

B-5 CALCULATION

M1 M2Pigment, percent by mass = ------------- X 100

S

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Where,M1= Mass of the tube plus pigment,M2 =Mass of the tubeS =Mass of the paint sample taken.

A N N E X C(Refer clause 3.1)

DETERMINATION OF PHOSPHORUS CONTENT IN PIGMENT

C-1 OUTLINE OF METHOD

The paint contains active ingredients such as ammonium polyphosphate, penta erythritol,dicynadiamide and titanium dioxide. After separation of pigments, the phosphorus content isdetermined by the following method.

C-2 APPARATUS

C-2.1 Analytical balance, Least Count 0.1mg

C-2.2 Heating oven capable to maintain 150C, Least count 2CC-2.3 Muffle furnace of range upto 1200C

C-2 REAGENTS

C-2.1 Citric Acid

C-2.2 Ammonia solution

C-2.3 Phenolphthalein as iondicator

C-2.4 Magnesium chloride (MgCl2, 6 H2O)

C-2.5 Ammonium chloride

C-2.6 Hydrochloric AcidC-3 PROCEDURE

C-3.1 Preparation of Ammonium Citrate solution -Neutralise 200 gm of Citric Acid withabout 350 ml of strong ammonia using phenolphthalein as Indicator.

C-3.2 Preparation of Magnesia Mixture- Dissolve 25 gm of Magnesium chloride (MgCl2, 6H2O) and 50 gm of ammonium chloride in 250 ml of water and add slight excess of ammoniasolution. Allow to stand overnight and filter it, if a precipitate is present. Acidify with dilute HCland add 1ml conc. HCl and make the volume to 500 ml with distilled water.

C-3.3 Take exactly weighed 5 gms of pigment in a 250 ml beaker and digeste for about half anhour with 50 ml of water, 20 ml. of conc. HCl and 5 ml of conc.HNO3. Then heat it almost to

dryness on a sand bath and later bake in an oven for about half an hour at 110 C. Cool thebeaker and add dilute HCl (1:1) in thev cooled mass. Filter it. The precipitate is thoroughlywashed with hot water and the filtrate made up to 500 ml. Take 50 ml filtrated solution and add20 ml ammonium citrate, 50 ml water, 50ml liquor ammonia and 50 ml magnesia mixture. Stirthe solution vigorously for about 15 minutes and allowed to stand for over night. It is filtered andthe precipitate is washed with dilute Ammonia (1:3) until the filtrate is free from chloride test.Dry the precipitate in an oven for about one hour and then ignite at 1000Cin a muffle furnacefor about 4 hours in a pre-weighed crucible. Weigh the crucible after cooling in desicator.

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C-4 CALCULATION

Phosphorus, percent =(W1- W2) 55.85

where, W1 = weight of the crucible with residueW2 =weight of the empty crucible.

A N N E X D(Table 1, Sl No.12)

FIRE TEST FOR INTUMESCENT FIRE RETARDANT PAINT

D-1 OUT LINE OF THE METHOD

The apparatus consisting of a two foot tunnel inclined at 380 to the horizontal in which paintedpanel placed facing downwards to form the roof of the tunnel as shown in figure 2. Paint undertest should be applied at the recommended dry film thickness.

D-2 EVAL UATION OF THE COMPOSITIONS FOR FIRE TEST

D-2.1 2 foot-tunnel test

D-2.1.1 Apparatus - The frame of the tunnel is fabricated from 20 x 20 x 3 mm angle ironmounted on a 125 x 660 mm base plate. The sample holding rack utilises a 750 x 100 mmspecimen size. An asbestos backing plate of 750 x 100 is used to prevent the test specimen fromwarping during the fire test. A small opening at the lower end of the tunnel is provided with amirror to observe the propagation of the flame. Temperature at the back of the panel ismeasured by inserting thermocouple through a small hole at the top cover which is locatedright above the burner. A Bunsen burner is used at the lower end of the inclined tunnel and thedistance between the burner top and test specimen is about 40 mm.

D-2.1.2 Procedure

The paint is applied on the wooden panels (Himalayan fir) of size 750 x 100 x 10 mm. Three

coats of paint is applied to build up a film thickness of 500 25 microns and allowed to dry for 7days at ambient conditions. The panel is positioned in the inclined top and the asbestos platewhich is of the size of the test specimen is placed above the painted panel. Mark the coated panelin such a way that 0 mark is positioned exactly above the tip of the burner and further markingare made in 25 mm succession till end of the panel as shown in figure -1. Panel is exposed toflame for ten minutes with pressure 2.0 lbs / square inch and the following observations are to benoted.

(a) Char height: Maximum height of char in millimeter at a point directly above theburner.

(b) Flame spread length: Only flame extending along the surface of the test panel

should be recorded as flame spread length.

(c) After glow: The time in seconds for which panel emits light after the source offire is removed.

(d) After flaming: The time in seconds for which flame continues after removal of thesource of fire.

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0 1 2 3 4 5 6 7 8

4.0

273

Figure 1: Test panel for fire test

Figure 2: Fire test apparatus (2 Foot tunnel)