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American Dental Association Specification No. 8 for Zinc Phosphate Cement
REPORTS OF COUNCILS AND BUREAUS Revised American National Standards Institute/American Dental Association Specification No. 8 for Zinc Phosphate Cement Council on Dental Materials and Devices R e v is e d A m e r ic a n D e n ta l A s s o c ia tio n S p e c if ic a tio n N o . 8 fo r Z in c P h o s p h a te C e m e n t h a s b e e n a p p ro v ed b y th e C o u n c il o n D e n ta l M a te ria ls and D e v ic e s o f th e A m e r ic a n D e n ta l A s s o c ia tio n . T h e fo rm u la tio n o f th is and o th e r s p e c ific a tio n s fo r d en tal m a te ria ls and d e v ic e s is b ein g ca rrie d o n th rou gh s u b c o m m itte e s o f th e A m e ric a n N a tio n a l S ta n d a rd s C o m m itte e M D 1 5 6 fo r D e n ta l M a te ria ls an d D e v ic e s . T h e C o u n c il on D e n ta l M a te ria ls and D e v ic e s a c ts a s th e a d m in istra tiv e s p o n so r o f th a t c o m m itte e , w h ich h a s re p re s e n ta tio n fro m all in te re s ts in th e U n ite d S ta te s in th e sta n d a rd iz a tio n o f m a te ria ls , e q u ip m en t, and in s tru m e n ts in d e n tis try . T h e C o u n c il h a s ad op ted th e s p e c ific a tio n s sh ow in g p ro fe ss io n a l re c o g n i tio n o f th e ir u se fu ln e ss in d e n tistry an d h a s fo r w ard ed th e m to th e A m e ric a n N a tio n a l S ta n d a rd s In s titu te w ith a re co m m e n d a tio n th a t th e s p e c i fic a tio n s b e ap p ro v ed a s A m e ric a n N a tio n a l S ta n d a rd s . A p p ro v a l o f A D A S p e c ific a tio n N o . 8 a s an A m e r ic a n N a tio n a l S ta n d a rd w a s g ran ted b y th e A m e ric a n N a tio n a l S ta n d a rd s In stitu te on S e p t 15, 1977. T h e C o u n c il a ck n o w le d g e s , w ith th a n k s , the w o rk o f th e su b co m m itte e m e m b e rs w h o fo rm u lated th e stan d ard : R ic h a rd D . N o rm a n (c h a irm a n ), Jo h n s o n and Jo h n s o n , E a s t W in d s o r, N J ; Jo h n P o w e rs , U n i v e rsity o f M ic h ig a n , A n n A r b o r ; C h a rle s
F.
u ated co m p le te ly and o n ly m in im al c h a n g e s w ere m ad e. T h e s e in clu d ed th e up d ating o f th e In te rn a tio n a l S y s te m o f U n its , a sim p lify in g o f te s t m e th o d o lo g y , and a re q u ire m e n t fo r m a n u fa c tu re rs to s ta te th e p o w d er-liq u id ra tio th a t w ill b e u sed during th e te stin g o f th e c e m e n t. T h e s e c h a n g e s r e fle c t sim ila r tre n d s w ith o th e r s p e c ific a tio n s and w ill aid in th e o v era ll u s e fu ln e s s o f S p e c ific a tio n N o . 8.
R ev is e d A m e ric a n N atio n a l S ta n d a rd s In s titu te /A m e ric a n D en tal A ssociation S p e c ific a tio n N o. 8 fo r Zinc P h o sp h a te C em e n t (A pproved D ec e m b e r 1977 as A D A S pecificatio n)
1. Scope and classification This specification is for zinc phosphate cem ent, the primary uses o f which are to retain or to seal dental appliances to oral structures or to other appliances; to serve as a base or foundation for other filling material; and to serve as a temporary filling mate rial. 1.2 Types and classes. Z inc phosphate cement covered by this specification shall be o f two types. Type I: Fine particle size. Type I cem ent is designed for the accurate seating o f precision appliances and for other uses (1.1). T ype II: Medium particle size. Type II cem ent is recommended for all uses (1.1) except the cementing o f precision appliances.
1.1 Scop e.
Applicable specifications
B u rn s , S . S . W h ite C o ., K in g o f P ru s s ia , P a ; Jo s e p h P . M o ffa , U S P u b lic H e a lth S e r v ic e , S a n F r a n c is c o ; D . T im o th y W o lf, S ta r D e n ta l M fg . C o ., C o n s h o h o c k e n , P a .
R ea g en t C hem icals, Washing ton, D C , Am erican Chemical S ociety , 1960, p 9 shall apply to the test for arsenic (4.3.6). (T he most recent edition [fifth] o f R ea g en t C hem icals was published in 1975.)
T h e th ird re v isio n o f S p e c ific a tio n N o . 8 w as su b m itted and ap p rov ed to u p date and upgrade
Requirements T h e cem ent shall consist o f a powder and a liquid which, when mixed according to the manu facturer’s directions, will harden.
th e re q u ire m e n ts fo r d en tal z in c p h o sp h a te c e m e n t. E a c h s e c tio n o f th is s p e c ific a tio n w a s e v a l
2.1 Specifications.
3.
3.1 M aterial.
JADA, Vol. 96, January 1978 ■ 121
Table ■ Physical property requirements. Time of setting at Minimum 37 C (99 F) compressive _____ (minutes)_____ Strength (24 hours) Minimum Maximum 75 MN/m? (765.3 kg/cm?)
3.2 Liquid. 3.2.1 Condition.
T h e liquid shall be w ater-clear and there shall be no deposits or sediment on the inside o f the container, 3.2.2 V olum e. T h e liquid shall be supplied in an amount 20% in excess o f that necessary to com bine with the total amount o f powder in a container o f full portion size when mixed to the m anufacturer’s recom mended consistency. 3.3 Powder. 3.3.1 Condition. The powder shall be free o f ex traneous particles foreign to the material. T h e pigment shall be uniformly dispersed throughout the powder. 3.4 U n set cem ent. 3.4.1 Spatulation. Cem ents when spatulated a c cording to the manufacturer’s instructions shall not form lumps or granules or evolve gases. 3.5 S et cem ent. 3.5.1 C olor. Colors for the set cem ent shall be specified by the purchaser. 3.6 A rsenic content. T h e limitation on arsenic con tent shall be as listed in the Table. 3 .7 Physical properties. T h e requirements fo r time o f setting, com pressive strength, film thickness, and solubility and disintegration shall be as listed in the T able. 3 .8 Instructions. Instructions for proportioning and manipulation shall include information regarding temperature o f the slab, clinical powder-liquid ratio in grams per milliliter, rate o f incorporating the powder, time o f mixing, maximum working time betw een the end o f the mixing and the seating o f the appliance or any o ther use o f the cem ent, and instructions for proper storage o f the liquid after the immediate container has been opened. 4.
Sampling, inspection, and testing procedures T hree containers o f powder, prefer ably o f different shades, together with a corresponding number o f containers o f liquid shall be procured for testing for com pliance with this specification. 4.1.1 Pooling o f liquids. I f the liquid com plies with the requirements o f 3 .2 .1 , the contents o f the sample containers o f liquid shall be emptied into a clean glassstoppered bottle. 4.1.2 Pooling o f powders. I f the powder complies with the requirements o f 3 .3 .1 , the contents o f the sam ple containers o f powder shall be mixed together for use in 4.1 .3 . 4.1.3 Com posite samples. All tests, with the ex
4.1 Sampling.
Maximum film thickness (Mm)
Type I Type II 40 25
Maximum solubility and disintegration (24 hsurs) 0.2% by weight
Maximum arsenic content 0.0002% by weight (1:500,000)
ception o f those prescribed in 3.2.1 and 3.3.1 shall be conducted on specimens made from the com posite samples o f liquid and powder specified in 4.1.1 and 4 .1 .2 respectively. 4.2 Inspection. Visual inspection shall be used in determining com pliance with the requirements outlined in 3 .1 ; 3 .2 .1 -3 .3 .1 ; 3 .4 .1 ; 3 .5 .1 ; 3 .8 ; and 5. 4.3 Testing procedures. 4.3.1 Preparation o f test specimens. T h e prepara tion o f all test specimens shall be conducted at 23 ± 2 C and 5 0 ± 10% relative humidity. T h e powder-liquid ratio and mixing technique, as recommended by the manu facturer in section 3.8, shall be used to obtain the stan dard mix o f cem ent for the preparation o f all test spec imens. N o particles o f powder or any unused liquid shall remain on the slab when the mixing is completed. 4.3.2 Tim e o f setting. A ring held at room tempera ture and approximately 4.8 mm high and 11.1 mm out side diameter and 9.5 mm internal diameter shall be placed on a flat glass plate and filled with a portion o f the standard m ix o f cem ent. T h ree minutes after starting the mix, the specimen shall be transferred to an atm os phere o f 100% relative humidity at 37 C. T hree and a half minutes after beginning the mix, a standard Gillm ore needle, weighing 4.45 newtons (453.6 g) and having an end 1.06 mm in diameter, shall be carefully lowered vertically onto the horizontal surface o f the cem ent. This shall be repeated at half-minute intervals. T h e time o f setting is the number o f minutes elapsed from the starting o f the mix to the time when the needle fails to make a perceptible circle on the surface of the specimen when allowed to rest thereon under its own weight. T h e setting time shall be reported to the nearest minute. 4.3.3 Com pressive strength. T h e test specimens shall be cylinders 12 mm high and 6 mm in diameter. T h e ends o f the specimens shall be flat and smooth and shall be parallel to each other at right angles to the long axis o f the cylinder. A cylindrical mold 12 mm high and 6 mm in diameter shall be placed on a flat glass plate and slightly over filled with a portion o f the standard mix o f cem ent within three minutes after commencing the mixing. A second flat glass plate shall be pressed on top o f the mold. T h e mold and plates shall be held together firmly. A split mold may be used. All apparatuses shall be made o f a substance that will not react with the cement. T h e molds may be coated with a suitable mold-release material. T hree minutes after the start o f the mix, the cem ent in the mold shall be transferred to an atmo sphere o f 100% relative humidity at 37 C . One hour later
122 ■ REPORTS OF COUNCILS AND BUREAUS / JADA, Vol. 96, January 1978
the ends o f the cylinder shall be surfaced plane at right angles to the axis. The ends o f the cem ent cylinders may be ground flat by the use o f 240 grit silicon carbide paper. T h e test specimens shall be kept wet during the grinding. A fter surfacing, the specimens shall be removed from the mold and shall be immersed in distilled water at 37 C . The time lapse between the start o f the mixing and the crushing shall be 24 hours. A small piece o f blotting paper (approximately 0.5 mm thick) wet with water shall be inserted between the ends o f the specimen and the platens o f the testing machine. T he specimens shall be loaded at a head speed o f 0.05 cm/minute and shall be kept wet during the test. T h e value for com pressive strength shall be reported as the average o f three or more from a lot o f five speci mens and shall be rounded off to the nearest 1 MN/m2. If the values for individual specimens fall more than 15% below the average o f the five, they shall be dis carded and the average o f the remaining specimens shall be reported. If more than two o f the specimens are eliminated, the test shall be repeated. 4.3.4 Film thickness. A portion o f the standard mix o f cem ent shall be placed between two flat square or round glass plates o f uniform thickness. T he surface areas o f the plates between which the cem ent is spread shall be approximately 2 sq cm. Three minutes after the mix is started, a load o f 14.7 newtons (15 kg) shall be applied vertically on the top plate. T en minutes after the mix is started, the thickness o f the two plates with the cem ent film between them shall be determined. T h e difference in the thickness o f the plates with and with out the cem ent film shall be considered as the film thickness. An average o f three tests shall be reported to the nearest 5/xm. 4.3.5 Solubility and disintegration. O ne-half milli liter o f a standard mix o f cem ent shall be placed in a split stainless steel ring (inside diameter 20 mm and 1.5 mm thick) that is sitting on a thin, polyethylene sheet backed by a flat plate. A nother flat plate faced with a sheet o f thin polyethylene shall be used to press the cem ent into the ring. When the specimens are formed, a piece o f fine platinum or corrosion-resistant wire shall be placed in the soft cem ent to provide a convenient means o f holding the specimens. T hree minutes after the mix is started, the plates and cem ent shall be placed for one hour in an atmosphere having a relative humid ity o f 100% at 37 C. A fter one hour, the specimens shall be withdrawn from the oven and two specimens shall be placed in each tared weighing bottle and weighed. T h e combined weight o f the two specimens and the weighing bottle, less the weight of weighing bottle and the platinum wire, shall be taken as the weight o f the specimens o f cem ent. T he specimens shall be submerged immediately by pouring 50 ml o f distilled water into the weighing bottle, which shall be stored for 23 hours at 37 C . The speci mens shall then be removed from the water. T here shall
be no evidence o f crystal growth on the surface o f the specimens. T h e water shall be evaporated from the weighing bottle at a temperature ju st below 100 C . T he weighing bottle shall then be dried at 150 C to constant weight. A fter cooling to room temperature in a desic cator containing thoroughly dry anhydrous calcium sul fate (C a S O i) or silica gel (freshly dried at 130 C ), the weighing bottle and contents shall be weighed with a precision o f 0.2 mg. T his cy cle o f heating the weighing bottle to 150 C , cooling over a desiccant, and reweigh ing shall be repeated until the weight loss o f each bottle is not more than 0.5 mg in any 24-hour period. T he difference between the final weight o f the weighing bottle and its initial weight shall be the amount o f disin tegration. T h e gain in weight divided by the weight o f the specimens times 100 gives the percentage o f inte gration. T h e average o f duplicate tests (two weighing bottles containing two specimens each) shall be re ported to the nearest 0.1% . 4.3.6 A rsenic content. O ne gram o f hardened ce ment, obtained from a specimen 24 hours old that has been stored in a dry, air-tight container, shall be pow dered to pass a no. 200 sieve. T h e powdered sample shall be digested in 100 ml o f distilled water on a steam bath for one hour. The filtrate shall be used in the test for water-soluble arsenic. The test for arsenic shall conform to that designated in R ea g en t Chem icals, Am erican Chem ical Society Specifications (2.1) or to an analytical technique o f similar precision. 5. Preparation for delivery 5.1 Packaging. T h e cem ent powder and liquid shall be supplied in properly sealed containers made o f mate rials that shall not contam inate or permit contamination o f the contents. 5.2 Instructions. Instructions for use shall accom pany each package and shall include information as stated in section 3.8. 5 J Marking. 5.3.1 Lot numbers. Each immediate container o f powder and each container o f liquid shall be marked with a serial number or a com bination o f numbers that shall refer to the m anufacturer’s records for that par ticular lot or batch o f cem ent powder or liquid. 5.3.2 D ate o f manufacture. T h e date o f manufac ture shall be indicated clearly by a six-digit number marked on the package or container in which the mate rial is prepared for retail marketing. T h e first two digits shall indicate the month, the second two the day, and the third two the year. 5.3.3 N et weight and volume. T h e net weight in grams o f the powder shall be indicated on the container. T h e net volume of the liquid in milliliters shall be indi cated on the container. 5.3.4 Identification o f type. The external surface o f the package in which the cem ent powder is packaged for retail marketing shall indicate the purpose or pur poses for which the material is intended (1.2).
REPORTS OF COUNCILS AND BUREAUS / JADA, Vol. 96, January 1978 ■ 123
F.
u ated co m p le te ly and o n ly m in im al c h a n g e s w ere m ad e. T h e s e in clu d ed th e up d ating o f th e In te rn a tio n a l S y s te m o f U n its , a sim p lify in g o f te s t m e th o d o lo g y , and a re q u ire m e n t fo r m a n u fa c tu re rs to s ta te th e p o w d er-liq u id ra tio th a t w ill b e u sed during th e te stin g o f th e c e m e n t. T h e s e c h a n g e s r e fle c t sim ila r tre n d s w ith o th e r s p e c ific a tio n s and w ill aid in th e o v era ll u s e fu ln e s s o f S p e c ific a tio n N o . 8.
R ev is e d A m e ric a n N atio n a l S ta n d a rd s In s titu te /A m e ric a n D en tal A ssociation S p e c ific a tio n N o. 8 fo r Zinc P h o sp h a te C em e n t (A pproved D ec e m b e r 1977 as A D A S pecificatio n)
1. Scope and classification This specification is for zinc phosphate cem ent, the primary uses o f which are to retain or to seal dental appliances to oral structures or to other appliances; to serve as a base or foundation for other filling material; and to serve as a temporary filling mate rial. 1.2 Types and classes. Z inc phosphate cement covered by this specification shall be o f two types. Type I: Fine particle size. Type I cem ent is designed for the accurate seating o f precision appliances and for other uses (1.1). T ype II: Medium particle size. Type II cem ent is recommended for all uses (1.1) except the cementing o f precision appliances.
1.1 Scop e.
Applicable specifications
B u rn s , S . S . W h ite C o ., K in g o f P ru s s ia , P a ; Jo s e p h P . M o ffa , U S P u b lic H e a lth S e r v ic e , S a n F r a n c is c o ; D . T im o th y W o lf, S ta r D e n ta l M fg . C o ., C o n s h o h o c k e n , P a .
R ea g en t C hem icals, Washing ton, D C , Am erican Chemical S ociety , 1960, p 9 shall apply to the test for arsenic (4.3.6). (T he most recent edition [fifth] o f R ea g en t C hem icals was published in 1975.)
T h e th ird re v isio n o f S p e c ific a tio n N o . 8 w as su b m itted and ap p rov ed to u p date and upgrade
Requirements T h e cem ent shall consist o f a powder and a liquid which, when mixed according to the manu facturer’s directions, will harden.
th e re q u ire m e n ts fo r d en tal z in c p h o sp h a te c e m e n t. E a c h s e c tio n o f th is s p e c ific a tio n w a s e v a l
2.1 Specifications.
3.
3.1 M aterial.
JADA, Vol. 96, January 1978 ■ 121
Table ■ Physical property requirements. Time of setting at Minimum 37 C (99 F) compressive _____ (minutes)_____ Strength (24 hours) Minimum Maximum 75 MN/m? (765.3 kg/cm?)
3.2 Liquid. 3.2.1 Condition.
T h e liquid shall be w ater-clear and there shall be no deposits or sediment on the inside o f the container, 3.2.2 V olum e. T h e liquid shall be supplied in an amount 20% in excess o f that necessary to com bine with the total amount o f powder in a container o f full portion size when mixed to the m anufacturer’s recom mended consistency. 3.3 Powder. 3.3.1 Condition. The powder shall be free o f ex traneous particles foreign to the material. T h e pigment shall be uniformly dispersed throughout the powder. 3.4 U n set cem ent. 3.4.1 Spatulation. Cem ents when spatulated a c cording to the manufacturer’s instructions shall not form lumps or granules or evolve gases. 3.5 S et cem ent. 3.5.1 C olor. Colors for the set cem ent shall be specified by the purchaser. 3.6 A rsenic content. T h e limitation on arsenic con tent shall be as listed in the Table. 3 .7 Physical properties. T h e requirements fo r time o f setting, com pressive strength, film thickness, and solubility and disintegration shall be as listed in the T able. 3 .8 Instructions. Instructions for proportioning and manipulation shall include information regarding temperature o f the slab, clinical powder-liquid ratio in grams per milliliter, rate o f incorporating the powder, time o f mixing, maximum working time betw een the end o f the mixing and the seating o f the appliance or any o ther use o f the cem ent, and instructions for proper storage o f the liquid after the immediate container has been opened. 4.
Sampling, inspection, and testing procedures T hree containers o f powder, prefer ably o f different shades, together with a corresponding number o f containers o f liquid shall be procured for testing for com pliance with this specification. 4.1.1 Pooling o f liquids. I f the liquid com plies with the requirements o f 3 .2 .1 , the contents o f the sample containers o f liquid shall be emptied into a clean glassstoppered bottle. 4.1.2 Pooling o f powders. I f the powder complies with the requirements o f 3 .3 .1 , the contents o f the sam ple containers o f powder shall be mixed together for use in 4.1 .3 . 4.1.3 Com posite samples. All tests, with the ex
4.1 Sampling.
Maximum film thickness (Mm)
Type I Type II 40 25
Maximum solubility and disintegration (24 hsurs) 0.2% by weight
Maximum arsenic content 0.0002% by weight (1:500,000)
ception o f those prescribed in 3.2.1 and 3.3.1 shall be conducted on specimens made from the com posite samples o f liquid and powder specified in 4.1.1 and 4 .1 .2 respectively. 4.2 Inspection. Visual inspection shall be used in determining com pliance with the requirements outlined in 3 .1 ; 3 .2 .1 -3 .3 .1 ; 3 .4 .1 ; 3 .5 .1 ; 3 .8 ; and 5. 4.3 Testing procedures. 4.3.1 Preparation o f test specimens. T h e prepara tion o f all test specimens shall be conducted at 23 ± 2 C and 5 0 ± 10% relative humidity. T h e powder-liquid ratio and mixing technique, as recommended by the manu facturer in section 3.8, shall be used to obtain the stan dard mix o f cem ent for the preparation o f all test spec imens. N o particles o f powder or any unused liquid shall remain on the slab when the mixing is completed. 4.3.2 Tim e o f setting. A ring held at room tempera ture and approximately 4.8 mm high and 11.1 mm out side diameter and 9.5 mm internal diameter shall be placed on a flat glass plate and filled with a portion o f the standard m ix o f cem ent. T h ree minutes after starting the mix, the specimen shall be transferred to an atm os phere o f 100% relative humidity at 37 C. T hree and a half minutes after beginning the mix, a standard Gillm ore needle, weighing 4.45 newtons (453.6 g) and having an end 1.06 mm in diameter, shall be carefully lowered vertically onto the horizontal surface o f the cem ent. This shall be repeated at half-minute intervals. T h e time o f setting is the number o f minutes elapsed from the starting o f the mix to the time when the needle fails to make a perceptible circle on the surface of the specimen when allowed to rest thereon under its own weight. T h e setting time shall be reported to the nearest minute. 4.3.3 Com pressive strength. T h e test specimens shall be cylinders 12 mm high and 6 mm in diameter. T h e ends o f the specimens shall be flat and smooth and shall be parallel to each other at right angles to the long axis o f the cylinder. A cylindrical mold 12 mm high and 6 mm in diameter shall be placed on a flat glass plate and slightly over filled with a portion o f the standard mix o f cem ent within three minutes after commencing the mixing. A second flat glass plate shall be pressed on top o f the mold. T h e mold and plates shall be held together firmly. A split mold may be used. All apparatuses shall be made o f a substance that will not react with the cement. T h e molds may be coated with a suitable mold-release material. T hree minutes after the start o f the mix, the cem ent in the mold shall be transferred to an atmo sphere o f 100% relative humidity at 37 C . One hour later
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the ends o f the cylinder shall be surfaced plane at right angles to the axis. The ends o f the cem ent cylinders may be ground flat by the use o f 240 grit silicon carbide paper. T h e test specimens shall be kept wet during the grinding. A fter surfacing, the specimens shall be removed from the mold and shall be immersed in distilled water at 37 C . The time lapse between the start o f the mixing and the crushing shall be 24 hours. A small piece o f blotting paper (approximately 0.5 mm thick) wet with water shall be inserted between the ends o f the specimen and the platens o f the testing machine. T he specimens shall be loaded at a head speed o f 0.05 cm/minute and shall be kept wet during the test. T h e value for com pressive strength shall be reported as the average o f three or more from a lot o f five speci mens and shall be rounded off to the nearest 1 MN/m2. If the values for individual specimens fall more than 15% below the average o f the five, they shall be dis carded and the average o f the remaining specimens shall be reported. If more than two o f the specimens are eliminated, the test shall be repeated. 4.3.4 Film thickness. A portion o f the standard mix o f cem ent shall be placed between two flat square or round glass plates o f uniform thickness. T he surface areas o f the plates between which the cem ent is spread shall be approximately 2 sq cm. Three minutes after the mix is started, a load o f 14.7 newtons (15 kg) shall be applied vertically on the top plate. T en minutes after the mix is started, the thickness o f the two plates with the cem ent film between them shall be determined. T h e difference in the thickness o f the plates with and with out the cem ent film shall be considered as the film thickness. An average o f three tests shall be reported to the nearest 5/xm. 4.3.5 Solubility and disintegration. O ne-half milli liter o f a standard mix o f cem ent shall be placed in a split stainless steel ring (inside diameter 20 mm and 1.5 mm thick) that is sitting on a thin, polyethylene sheet backed by a flat plate. A nother flat plate faced with a sheet o f thin polyethylene shall be used to press the cem ent into the ring. When the specimens are formed, a piece o f fine platinum or corrosion-resistant wire shall be placed in the soft cem ent to provide a convenient means o f holding the specimens. T hree minutes after the mix is started, the plates and cem ent shall be placed for one hour in an atmosphere having a relative humid ity o f 100% at 37 C. A fter one hour, the specimens shall be withdrawn from the oven and two specimens shall be placed in each tared weighing bottle and weighed. T h e combined weight o f the two specimens and the weighing bottle, less the weight of weighing bottle and the platinum wire, shall be taken as the weight o f the specimens o f cem ent. T he specimens shall be submerged immediately by pouring 50 ml o f distilled water into the weighing bottle, which shall be stored for 23 hours at 37 C . The speci mens shall then be removed from the water. T here shall
be no evidence o f crystal growth on the surface o f the specimens. T h e water shall be evaporated from the weighing bottle at a temperature ju st below 100 C . T he weighing bottle shall then be dried at 150 C to constant weight. A fter cooling to room temperature in a desic cator containing thoroughly dry anhydrous calcium sul fate (C a S O i) or silica gel (freshly dried at 130 C ), the weighing bottle and contents shall be weighed with a precision o f 0.2 mg. T his cy cle o f heating the weighing bottle to 150 C , cooling over a desiccant, and reweigh ing shall be repeated until the weight loss o f each bottle is not more than 0.5 mg in any 24-hour period. T he difference between the final weight o f the weighing bottle and its initial weight shall be the amount o f disin tegration. T h e gain in weight divided by the weight o f the specimens times 100 gives the percentage o f inte gration. T h e average o f duplicate tests (two weighing bottles containing two specimens each) shall be re ported to the nearest 0.1% . 4.3.6 A rsenic content. O ne gram o f hardened ce ment, obtained from a specimen 24 hours old that has been stored in a dry, air-tight container, shall be pow dered to pass a no. 200 sieve. T h e powdered sample shall be digested in 100 ml o f distilled water on a steam bath for one hour. The filtrate shall be used in the test for water-soluble arsenic. The test for arsenic shall conform to that designated in R ea g en t Chem icals, Am erican Chem ical Society Specifications (2.1) or to an analytical technique o f similar precision. 5. Preparation for delivery 5.1 Packaging. T h e cem ent powder and liquid shall be supplied in properly sealed containers made o f mate rials that shall not contam inate or permit contamination o f the contents. 5.2 Instructions. Instructions for use shall accom pany each package and shall include information as stated in section 3.8. 5 J Marking. 5.3.1 Lot numbers. Each immediate container o f powder and each container o f liquid shall be marked with a serial number or a com bination o f numbers that shall refer to the m anufacturer’s records for that par ticular lot or batch o f cem ent powder or liquid. 5.3.2 D ate o f manufacture. T h e date o f manufac ture shall be indicated clearly by a six-digit number marked on the package or container in which the mate rial is prepared for retail marketing. T h e first two digits shall indicate the month, the second two the day, and the third two the year. 5.3.3 N et weight and volume. T h e net weight in grams o f the powder shall be indicated on the container. T h e net volume of the liquid in milliliters shall be indi cated on the container. 5.3.4 Identification o f type. The external surface o f the package in which the cem ent powder is packaged for retail marketing shall indicate the purpose or pur poses for which the material is intended (1.2).
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