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IS 15895 (2011): High Alumina Refractory Cement [MTD 15:Refractories]

IS 15895 : 2011

© BIS 2011

May 2011 Price Group 3

B U R E A U O F I N D I A N S T A N D A R D SMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

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Indian StandardHIGH ALUMINA REFRACTORY CEMENT —

SPECIFICATION

ICS 81.080

Refractories Sectional Committee, MTD 15

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the RefractoriesSectional Committee had been approved by the Metallurgical Engineering Division Council.

High alumina refractory cement (HAC) are essentially those, which contain calcium aluminates as primaryhydraulic constituent. Among the calcium aluminate phases monocalcium aluminate (CaO.Al2O3) is the mostdesirable one since it imparts both high early strength as well as high refractoriness. Calcium di-aluminate(CaO.2Al2O3) also is the other desirable calcium aluminate phase in HAC, though its hydration rate issignificantly slower compared to monocalcium aluminate. In some of the varieties of HAC, the presence ofnon-hydraulic phases like gehlenite (2CaO.2Al2O3.SiO2), perovskite (CaO.TiO2) are of common occurrence.These products are produced either by fusion or sintering process.

These cements are produced either by fusion or sintering process using a mix of calcareous material like limestone/hydrated lime/dolomitic lime stone and argillaceous material like Bauxite/Brown or white fused alumina/calcined alumina.

High alumina refractory cement (HAC) are categorized in 2 classes depending on their impurity content,namely, medium purity and high purity. High purity HACs are those whose total impurity content, that is SiO2+ TiO2 + Fe2O3 + MgO, does not exceed 2.0 percent. The impurity level of the product is controlled byappropriate selection of the raw materials. The alumina content of the medium purity is normally less than 50percent. The high purity grade HACs, like medium purity grade, can have varied range of alumina. The typicalchemical as well as physical properties of the various grades of medium and high purity HACs are given inTable 1.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value,observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance withIS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained inthe rounded off value should be the same as that of the specified value in this standard.

IS 15895 : 2011

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Indian StandardHIGH ALUMINA REFRACTORY CEMENT —

SPECIFICATION1 SCOPE

This standard covers the classification, evaluationprocedure and properties of HACs of high aluminarefractory cement.

2 REFERENCES

The standards listed below contain provisions,which through reference in this text, constituteprovisions of this standard. At the time ofpublication, the editions indicated were valid. Allstandards are subject to revision and parties toagreement based on this standard are encouraged toinvestigate the possibility of applying the mostrecent editions of the standards indicated below:

IS No. Title

650 : 1991 Specification for standard sandfor testing of cement (secondrevision)

1528 Methods of sampling andphysical tests for refractorymaterials:

(Part 1) : 2009 Determination of pyrometriccone equivalent (PCE) orsoftening point (third revision)

(Part 4) : 1974 Determination of cold crushingstrength (first revision)

4031 (Part 2) : 1999 Methods of physical tests forhydraulic cement: Part 2Determination of fineness byspecific surface by blaine airpermeability method (secondrevision)

4032 : 1985 Methods of chemical analysis ofhydraulic cement (first revision)

5513 : 1996 Specification for vicat apparatus(second revision)

10080 : 1982 Specification for vibrationmachine

12107 Methods of chemical analysis ofalumino-sil icate refractorymaterials:

(Part 1) : 1987 Determination of loss on ignition(Part 3) : 1987 Determination of aluminium(Part 5) : 1987 Determination of titanium(Part 6) : 1987 Determination of iron

3 SAMPLING

3.1 Samples for Testing and by Whom to be Taken

A sample or samples for testing may be taken by thepurchaser or his representative, or by any personappointed to superintend the works for the purposeof which the cement is required, or by hisrepresentative, or by any expert analyst employedor instructed by such purchaser or person, or by therepresentative of such expert analyst.

In any consignment of the container/bags, holdingrefractory cements of the same type and grade,manufactured by the same firm under similarconditions of productions, shall be grouped togetherto constitute a lot. The maximum size of any lot,however, shall be limited to 50 tonne.

3.2 Samples for Testing and How to be Taken

Each sample for testing shall consist of a mixture ofapproximately equal portions selected from at leasttwelve different positions in the heap or heaps whenthe cement is loose, or from not less than twelvedifferent bags, barrels or other packages, when thecement is not loose, or where there is a less numberthan twelve different bags, barrels or other packages,then from each bag, barrel or other package. Everycare shall be taken in the selection, to obtain a fairaverage sample. The final sample shall weigh at least5 kg.

3.3 Sampling Large Quantities

When more than 130 tonne of cement is to be sampledat one time, separate samples shall be taken fromeach 130 tonne or part thereof.

Not more than 130 tonne shall be stored in such amanner that it cannot be separately identified andsampled in accordance with the provisions of thisclause and be separated in bulk from the remainder.If more than 130 tonne of cement is stored in a silo,provision shall be made by which each 130 tonne orany part of 130 tonne in excess thereof, shall beisolated from the remainder and sampled at differentpoints.

4 TESTS

The sample or samples taken, as described in 3 shallbe tested in the manner specified for:

a) Pyrometric cone equivalent (PCE),

IS 15895 : 2011

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b) Fineness,c) Chemical composition,d) Strength, ande) Setting time.

4.1 Pyrometric Cone Equivalent

The cement shall be tested for refractoriness byIS 1528 (Part 1). The PCE of various grades of HACsare given in Table 1.

4.2 Fineness

The cement shall be tested for fineness by IS 4031(Part 2). The finenesses of various grades of HACsare given in Table 1.

4.3 Chemical Composition

The cement shall be tested for i ts chemicalcomposition as per the procedure prescribed inIS 4032, IS 12107 (Part 1), IS 12107 (Part 3), IS 12107(Part 5) and IS 12107 (Part 6).

The chemical compositions of various grades ofHACs are given in Table 1.

NOTE — Alternatively, XRF cana be used if agreed tobetween purchaser and manufacturer.

4.4 Strength

The average compressive strength of three cubes,prepared, stored and tested in the manner describedin Annex A. The strength data for various grades of

cements at the following stages of curing are givenin Table 1.

a) Strength after curing for one day, that is 24 ±½ h, are measured for both medium as well ashigh purity HACs.

b) The strength after curing for three days, thatis 72 ± 1 h, is measured for medium purityHACs.

c) Strength after curing for one day andsubsequently for one day at 110oC, normallytermed as 1 + 1 day strength, is measured forhigh purity HACs.

4.5 Setting Time

The setting time of the cement, when tested by themethod described in Annex B and their values fordifferent grades of HACs are given in Table 1.

5 STORAGE

The cement shall be stored in such a manner as topermit of easy access for proper inspection and in asuitable weather-tight package to protect the cementfrom hydration and to minimize loss during transport.The storage life should not be less than six months.

6 MANUFACTURER’S CERTIFICATE

The manufacturer shall satisfy himself that thecement conforms to the requirements of thisstandard, if requested, shall furnish a certificate tothis effect to the purchaser or his representative.

Table 1 Characteristic of the HACs(Forword; and Clauses 4.1, 4.2, 4.3, 4.4 and 4.5)

Sl No. Characteristics Medium Purity High Purity

Grade I Grade II (1) (2) (3) (4) (5) i) Chemical Constituents:

a) Al2O3 percent, Min 45 69, Min 78b) SiO2 percent, Max 6.5 1 .2 1c) Fe2O3, Max 7 0 .3 0 .3d) TiO2, Max 7 Trace Tracee) CaO, Max 34 30, Max 20f) MgO (typical) 1 0 .6 0 .4

ii) CCS (kg/cm2) of 1 : 3vibrated mortar usingstandard graded sand:

a) After 1 day 300, Min 330, Min 150, Minb) After 1 day + 1 day at 110 °C — 500, Min 400, Minc) at 3 days 380, Min — —

iii) Specific surface area(cm2/gm), Min 3 000 3 500 4 000

iv) Setting time, Min:a) Initial 30, Min 30, Min 30, Minb) Final 400, Max 400, Max 400, Max

v) Refractoriness: Orton/°C, Min 12/1337 31/168320- 35/1785

30/1564-1683

IS 15895 : 2011

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ANNEX A(Clause 4.4)

DETERMINATION OF COMPRESSIVE STRENGTH OF HIGH ALUMINA REFRACTORY CEMENT

A-1 TEMPERATURE AND HUMIDITY

The temperature of moulding room, shall bemaintained at 27 ± 2 ºC. The relative humidity of thelaboratory shall be 65 ± 5 percent.

The temperature of dry materials and water shall bemaintained at 18 ± 2°C. The curing chamber or moistroom shall be maintained at 18 ± 2 ºC and at a relativehumidity of 90 ± 5 percent.

A-2 GENERAL

A-2.1 Standard Sand

The standard sand to be used in the test shallconform to IS 650.

A-3 APPARATUS

A-3.1 Vibration Machine — Vibration machine shallconform to IS 10080.

A-3.2 Poking Rod — Poking rod shall conform toIS 10080.

A-3.3 Cube Mould — The mould shall be of 70.6 mmsize conforming to IS 10080.

A-3.4 Gauging Trowel — Gauging trowel shall havea steel blade 200 mm in length with straight edgesweighing 220 ± 10 g.

A-3.5 Balance — The balance shall conform to thefollowing requirement:

a) On a balance in use, the permissible variationat a load of 1 000 g shall be + 1.0 g. Thepermissible variation on new balance shall beone half of this value. The sensibili tyreciprocal shall be not greater than twice thepermissible variation.

NOTES

1 The sensibility reciprocal is generally defined asthe change in load required to change the position ofrest of the indicating element or elements at a nonautomatic indicating scale a definite amount of anyload.2 Self indicating balance with equivalent accuracymay also be used.

b) Graduated glass cylinders, of 100 to 250 mlcapacity — The permissible variation on thesecylinders shall be ±1 ml. The main graduationlines of the cylinders shall be in circles andshall be numbered. The least graduations shallextend at least one seventh of the way around,and intermediate graduations shall extend atleast one-fifth of the way around the cylinder.

The graduation lines may be omitted for thelowest 5 ml.

A-4 PREPARATION OF TEST SPECIMENS

A-4.1 Mix Proportions and Mixing

Clean appliances shall be used for mixing and thetemperature of the test room at the time when theabove operations are being performed shall be 27 ±2ºC. Potable/distilled water shall be used in preparingthe cubes. The temperature of dry materials and watershall be maintained at 18 ± 2°C

The material for each cube shall be mixed separatelyand the quantity of cement (one part), standard sand(three parts) and water shall be as follows:

a) Cement: 200 g,b) Standard sand: 600 g, andc) Water : 80 g.

Place on a nonporous plate, a mixture of cement andstandard sand. Mix it dry with a trowel for 1 min andthen with water until the mixture is of uniform colour10 percent, by weight of the sand, cement mortarmix, of water shall be used as specified above. Thetime of mixing shall in any event be not less than3 min and should the time taken to obtain a uniformcolour exceed 4 min, the mixture shall be rejected andthe operation repeated with a fresh quantity ofcement, sand and water.

A-4.2 Moulding Specimens

In assembling the moulds ready for use, cover thejoints between the halves of the mould with a thinfilm of petroleum jelly and apply a similar coating ofpetroleum jelly between the contact surfaces of thebottom of the mould and its base plate in order toensure that no water escapes during vibration. Treatthe interior faces of the mould with a thin coating ofmould oil.

Place the assembled mould on the table of thevibration machine and hold it firmly in position bymeans of a suitable clamp. Attach a hopper of suitablesize and shape securely at the top of the mould tofacilitate filling and this hopper shall not to beremoved until the completion of the vibration period.

Immediately after mixing the mortar in accordancewith above, place the mortar in the cube mould andpoke with the rod specified. The mortar shall be poked20 times in about 8 s to ensure elimination of entrainedair and honey combing. Place the remaining quantityof mortar in the hopper of the cube mould and poke

IS 15895 : 2011

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again as specified for the first layer and then compactthe mortar by vibration.

The period of vibration shall be two minutes at thespecified speed of 12 000 ± 400 vibration per minute.

At the end of vibration, remove the mould togetherwith the base plate from the machine and finish thetop surface of the cube in the mould by smoothingthe surface with the blade of a trowel. Six such cubesper lot should be cast for the purpose of evaluation.

A-4.3 Curing Specimens

A-4.3.1 Moderate Purity HAC

Keep the filled moulds in a closet maintained at 18 ±2oC and 90 ± 5 percent RH for 24 ± ½ h aftercompletion of vibration. At the end of that period,remove them from the moulds and immediatelysubmerge three of them in clean fresh water. The waterin which the cubes are submerged shall be renewedevery day and shall be maintained at a temperatureof 18 ± 2 ºC. The curing of the water submergedspecimens should be done for 48 ± 1 h. After theyhave been taken out and until they are broken, thecubes shall not be allowed to become dry.

A-4.3.2 High Purity HAC

Keep the filled moulds in a closet maintained at

B-1 TEMPERATURE AND HUMIDITY

The temperature of moulding room, dry materials andwater shall be maintained at 18 ± 2 ºC. The relativehumidity of the laboratory shall be 90 ± 5 percent.

B-2 APPARATUS

B-2.1 Vicat Apparatus — Vicat apparatus shallconform to IS 5513.

B-2.2 Balance — The balance shall conform to thefollowing requirements:

On a balance in use, the permissible variation at aload of 1 000 g shall be ± 1.0 g. The permissiblevariation on new balance shall be one half of thisvalue. The sensibility reciprocal shall be not greaterthan twice the permissible variation.

NOTES

1 The sensibility reciprocal is generally defined as thechange in load required to change the position of rest ofthe indicating element or elements at a non automaticindicating scale a definite amount of any load.

18 ± 2oC and 90 ± 5 percent relative humidity for24 ± ½ h after completion of vibration. At the end ofthat period, remove them from the moulds and keepthree of them in an oven which is maintained at 110 ±5oC for 24 ± ½ h.

A-5 TESTING

The sets of three cubes cured at various conditions,as mentioned in section 4, are evaluated for theircompressive strength as per IS 1528 (Part 4).

A-6 CALCULATION

The measured compressive strength of the cubesshall be calculated by dividing the maximum loadapplied to the cubes during the test by the cross-sectional area, calculated from the mean dimensionsof the section and shall be expressed to the nearest0.5 N/mm². In determining the compressive strength,do not consider specimens that are manifestly faulty,or that give strengths differing by more than 10percent from the average value of all the testspecimens. After discarding specimens or strengthvalues, if less than two strength values are left fordetermining the compressive strength at any givenperiod, a retest shall be made.

ANNEX B(Clause 4.5)

DETERMINATION OF INITIAL AND FINAL SETTINGTIMES OF HIGH ALUMINA REFRACTORY CEMENT

2 Self indicating balance with equivalent accuracy mayalso be used.

B-2.3 Gauging Trowel — Gauging trowel shall havea steel blade of 200 mm length with straight edgesweighing 220 ± 10 g.

B-3 PROCEDURE

B-3.1 Preparation of Test Block

Prepare a neat cement paste by gauging the cementwith required percentage of water by weight of thedry cement. Potable or distilled water shall be usedin preparing the paste. Start a stopwatch at theinstant when water is added to the cement. The watershould be maintained at 18 ± 2oC. The temperature ofthe gauging room shall be maintained at 18 ± 2oC and90 ± 5 percent relative humidity. The Vicat mouldwith a cement paste gauged as above, the mouldresting on a non-porous plate. Fill the mouldcompletely and smooth off the surface of the pastemaking it level with the top of the mould. The cementblock thus prepared in the mould is the test block.

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Immediately after moulding, place the test block inthe moist closet or moist room and allow it to remainthere except when determinations of time of settingare being made.

NOTES

1 Clean appliances shall be used for gauging.

2 All the apparatus shall be free from vibration during thetest.

3 Care shall be taken to keep the needle straight.

B-3.2 Determination of Initial Setting Time

Place the test block confined in the mould and restingon the non-porous plate, under the rod bearing theneedle, lower the needle gently until it comes incontact with the surface of the test block and quicklyrelease, allowing it to penetrate into the test block.In the beginning, the needle will completely piercethe test block. Repeat this procedure until the needle,when brought in contact with the test block andreleased as described above, fails to pierce the blockbeyond 5.0 ± 0.5 mm measured from the bottom ofthe mould. The period elapsing between the time

when water is added to the cement and the time atwhich the needle fails to pierce the test block to apoint 5.0 ± 0.5 mm measured from the bottom of themould shall be the initial setting time.

B-3.3 Determination of Final Setting Time

Replace the needle of the Vicat apparatus by theneedle with an annular attachment. The cement shallbe considered as finally set when, upon applyingthe needle gently to the surface of the test block, theneedle makes an impression thereon, while theattachment fails to do so. The period elapsingbetween the time when water is added to the cementand the time at which the needle makes an impressionon the surface of test block while the attachmentfails to do so shall be the final setting time. In theevent of a scum forming on the surface of the testblock, use the underside of the block for thedetermination.

B-4 REPORTING OF RESULTS

The results of initial and final setting time shall bereported to the nearest 5 min.

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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also reviewedperiodically; a standard along with amendments is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed, it is taken up for revision. Users of Indian Standardsshould ascertain that they are in possession of the latest amendments or edition by referring to the latest issue of‘BIS Catalogue’ and ‘Standards: Monthly Additions’.

This Indian Standard has been developed from Doc No. : MTD 15 (4857).

Amendments Issued Since Publication______________________________________________________________________________________

Amendment No. Date of Issue Text Affected______________________________________________________________________________________

______________________________________________________________________________________

______________________________________________________________________________________

______________________________________________________________________________________

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