SNI 15-2049-2004

Portland Cement1.Scope This standard covers the scope, normative references, terms and definitions, types and use, quality requirements, sampling method, test methods, the requirement of passing the test, packaging, labeling requirements, storage and transportation of portland cement. 2 . Normative ASTM C 114-00, Standard test methods for chemical analysis of hydraulic cement. ASTM C 109/109M-01, Standard test method for compressive strength of hydraulic cement mortar. ASTM C151-00, Standard test method for autoclave expansion of portland cement. ASTM C 186-98, Standard test method for heat of hydration of hydraulic cement. ASTM C 187-98, Standard test method for normal consistency of hydraulic cement. ASTM C 191-01a, Standard test method for time of setting of hydraulic cement by vicat needle. ASTM C 204-00, Standard test method for fineness of hydraulic cement by air permeability apparatus. ASTM C 115-96a, Standard test methods fineness of portland cement by turbidimeter. ASTM C 266-99, Standard test methods for time of setting of hydraulic cement paste by gillmore needles. ASTM C 451-99, Standard test methods for early stiffening of hydraulic cement (paste method.) ASTM C 185-01, Standard test method for air content of hydraulic cement mortar, ASTM C 778-00, Standard specification for standard sand. ASTM C 183-97, Standar practice for sampling and the amount of testing of hydraulic cement. ASTM C 430-96, Standard test for fineness of hydraulic cement by 45-m (No325) Sieve. ASTM C 670-03, Standard practice for preparing precision and bias statements for test Methods for construction materials.

3. Term and Definitions 3.1 Portland Cement

hydraulic cement produced by grinding portland slag cement, especially the consisting of hydraulic calcium silicates and are ground together with the material additional form of one or more crystalline forms of calcium sulfate compounds and may be added with other additives. 3.2 air content of hydraulic cement hydraulic cement containing a certain amount of extra air in the cause the air contained in the mortar within the limits specified in as measured by a method. 3.3 Pasta Cement mixture of cement and water either hardened or unhardened 3.4 false set quickly lose the plasticity of the cement paste, mortar or concrete 3.5 moist chamber an enclosed space for storage and hardening example pasta, mortar and concrete where temperatures and high relative humidity can be regulated 3.6 mortar consisting of a mixture of cement, fine aggregate and water either in a state hardened or unhardened 4.Types and Uses 4.1 Type I portland cement is for general use that does not require special requirements such as those required by other types. 4.2 Type II portland cement is in its use requires endurance the sulfate or moderate heat of hydration. 4.3 Type III portland cement requires the use of high strength in the early stages after the binding occurs. 4.4 Type IV portland cement is in use requires the heat of hydration lower. 4.5 Type V portland cement is in its use requires endurance height to sulfate. 5 Terms of quality 5.1 Chemical requirements of portland cement shall meet the following requirements: Table 1 The main chemical conditions Unit in

No. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Commentary I SiO2, minimum Al2O3, maksimum Fe2O3, maksimum MgO, maksimum SO3, maksimum If C3A < 8,0 If C3A > 8,0 Lost incandescent,maksimum Insoluble Part, maksimum C3S, maksimuma) C2S, minimuma) C3A, maksimuma) C4AF + 2C3A or a) C4AF + C2F, maksimum 6,0 3,0 3,5 5,0 3,0 II

Type Portland cement III IV 6,0 6,0 3,5 4,5 3,0 1,5 15 2,3d)

V 6,0 2,3d)

20,0 b,c) 6,0 6,0 b,c) 6,0 3,0d)

6,5

3,0 1,5 8,0 -

2,5 1,5 35b) 40b) 7b) -

3,0 1,5 5b) 25c)

Note :a)

Terms restrictions chemically based calculations for potential compounds certain not to be construed that the oxide C = CaO, S = SiO2, A = Al2O3, F = Fe2O3, example C3A = 3CaO.Al2O3.

of potential compounds in pure state.

Titanium dioksida (TiO2) and Fosfor pentaoksida (P2O5) included in Al2O3 Value used to calculate the compound Al2O3 in potential (eg: C3A) for the purpose of the specification is the amount of precipitate obtained by the addition of NH4OH reduced the amount of Fe2O3 (R2O3 - Fe2O3) were obtained in the chemical analysis wet. When % Al2O3 0,64 , the percentage C3S, C2S, C3A and C4AF calculated as follows % Fe2O3

C3S = 3CaO.SiO2 = (4,071 x % CaO) (7,600 x %SiO2) (6,718 x % Al2O3) (1,430 x % Fe2O3) (2,852 x % SO3) C2S = 2CaO.SiO2 = (2,867 x %SiO2) (0,7544 x % C3S) C3A = 3CaO. Al2O3 = (2,650 x % Al2O3) (1,692 x % Fe2O3) C4AF = 4CaO. Al2O3.Fe2O3 = (3,043 x % Fe2O3) When % Al2O3 < 0,64 , formed solid solution ( C4AF + C2F) = 4CaO. Al2O3.Fe2O3 % Fe2O3 soC4AF+ C2Fand C3S calculated as follows : Cement with this composition contained therein are not C3A. C2S equipment is computed using the formula above: Calculations for all potential compounds is based on the determination of the oxide is calculated to close as possible to 0.1%. All calculation results are reported as close as possible with 1.0%.

b)

If the heat of hydration is required as listed in table terms additional physics (Table 4), the chemical condition does If the expansion is required because the sulfate listed in the table Additional physical requirements (Table 4), the Can not be used Table 2 Additional chemical requirement a) No Commentary I 1. 2. 3. 4. C3A, maksimum C3A, minimum (C3S + 2 C3A) , maksimum Alkali as (Na2O + 0,658 K2O), maksimum 0,60 C) Unit in Type Portland Cement II 58 b) 0,60 C) III 8 5 0,60 C) IV 0,60 C) V 0,60 C)

not apply.c)

chemical condition does not applyd)

Note a Additional chemical requirement applies only specifically required b Same as description for b) the terms of the main chemicals. c Only applicable if the cement used in concrete aggregate reactive to alkali.

5.2 Terms physics portland cement shall meet the following requirements: Table 3 The main physical requirements No . 1. Commentary Type Portland Cement I Fineness air permeability testm2/kg with tools Turbidimeter, min Blaine, min 2. Immortality: The autoclave expansionmaks 160 280 0,8 160 280 0,8 160 280 0,8 160 280 0,8 160 280 0,8 II III IV V

0 3. strong press Age 1 dayKg/cm2minimum Age 3 dayKg/cm2minimum Age 7 dayKg/cm2minimum Age 28 daykg/cm2, minimum 280 4. Bonding time (alternative methods) with the tool Gillmore -Start, minute, minimum - Finish, minute, maksimum Vicat - Start, minute, minimum - Finish, minute, maksimum Notea)

0

0

0

0

125

100 70a)

120 240

-

80

200

175 120a) -

-

70

150

-

170

210

60 600 45 375

60 600 45 375

60 600 45 375

60 600 45 375

60 600 45 375

Compressive strength requirement applies if the conditions of heat of hydration requirements as listed in the table additional physics (Table 4) or if the terms C3S + C3A requirements as listed in the table additional chemicals required (Table 2). Table 4 Additional physical requirementsa) No . 1. 2. Commentary I Binding of apparent penetration of the end minimum Hydration heat Age 7 daykal/gramma ks 50 Type Portland Cement II 50 III 50 IV 50 V 50

-

70b)

-

60

-

3.

Age 28 daykal/gramma ks compressive strength Age 28 dayKg/cm2 minimum

-

-

-

70

-

12

280 220b) 12

12

12

0,040 12

4.

expansion due to sulfate 14 daymaksimum 5. Air content of mortar volumemaksimum Notea) b)

Additional physical requirement applies only if specifically requested. When the terms of heat of hydration is required, then the condition C3S + C3A as listed in additional chemical table (Table 2) is not required. Compressive strength requirement applies when the heat of hydration requirements as listed in the table Additional physical requirements (Table 4) or when the C3A + C3S requirements as listed in additional chemical requirements table (Table 2) required.

6 . Way Sampling 6.1 Description of terms specific to the standard way 6.1.1 Lot specific amount of cement that were submitted for inspection at any time particular. A lot can represent one or more bin filled cement sequence. One can also represent a lot of the contents of one or more units of transport removed from the same bin. 6.1.2 Adjustable sampling frequency Testing program is prepared for testing of only two examples cement obtained from any existing lot, and prepared for testing at a later stage usual, as described below. The program uses probability factor and is designed in such a way that if the test results from the second sample meets the requirements of the program, could means with 95% confidence level and less than 5% of the sample would be outside the specification limits. 6.2 Purpose and Use 6.2.1 Sampling procedures that have been described are intended for use in terms of sampling hydraulic cement, as it is produced and prepared for marketed. This procedure is not intended as a sampling procedures on surveillance

quality during the production process. Testing procedures that have been described include the number of samples for testing should performed and provide guidance in terms of making the report. 6.2.2 Most of the requirements and specifications required by the building construction is that hydraulic cement to be used in the work must meet requirements as stated in the purchase specification, such as specification of appropriate paragraph 5. If regulations or these specifications require sampling of cement produced the provisions given in clause 5.4.1 should be implemented. 6.3 Implementation Procedures 6.3.1 Implementation procedures include sampling and testing process with view to determining whether it meets the requirements of the cement sample specifications acceptance. Testing cement sample is done using a specific method to determine whether the test results obtained from the cement sample meets specifications and test results expressed as the basis for acceptance or rejection of the lot cement represented for example. 6.3.2 These results are not intended nor required that cement should be tested with using all the chemical and physical test methods specified in this standard. 6.4 The type and size of sample cement sampling 6.4.1 Sample quotes (grab sample) obtained from the cement conveyor belt, from bulk cement warehouse or ship bulk cement. Sample quotation can be derived from a continuous flow of cement in the intervening time 10 min by using automated sampling device called quote examples. Examples cited were taken at each of these time intervals, over a period of time should be combined into a composite sample, representative of cement produced during period of time. 6.4.2 All the semen samples, both sample quotation or composite sample weighting at least 5 kg. 6.4.3 Examples of cement should be packed in containers that are impermeable to air and water vapor which has been given a number on a regular basis and sequentially. 6.5 The time required to complete testing 6.5.1 Cement producers should prepare so that cement can be taken, for example, testing as early as possible before the time the test results required. So at least the applicable interval in paragraph 6.5.2 can be followed.

6.5.2 If these things had been done, the testing laboratory should be set up test results no later than the specified number of days after the time sampling. Table 5 sampling interval calibration Compressive strength (the age test, day) Chemical analysis, autoclave, normal consistency Vicat apparatus, the apparatus blaine fineness, fast rigid paste method. 2. 3. 4. 5. Compressive strength (test results 3 days) Compressive strength and heat of hydration (age 7 days of test results) Expansion due to sulfate (age test results 14 days) Compressive strength and heat of hydration (test results 28 days) 6.6 Sampling 6.6.1 Of the conveyor belt that is being supplied to the warehouse bulk cement. Take one example cited cement weighing at least 5 kg at intervals about 6 hours. 6.6.2 Sampling cement when moved Sampling of cement when cement warehouse is being moved from one bin to another bin. Take one example cited cement cement from the flow being moved, for every 400 tons of cement or multiples thereof, but not sampling be less than the examples quoted cement and combined to obtain sample composites. 10 14 21 35 8

NO. 1.

Lapse of time (days)

6.6.3 Another method of sampling If both the above sampling method can not be used, for example cement can obtained using one of the methods below: 1 ) From the warehouse bulk cement in the hole expenditure Take the example of semen from the hole expenditure at a constant flow of cement, up to sampling completed. Estimated amount of cement should have taken in tons using the formula:

with: d is the depth in meters of cement, which is above the hole expenses. If the cement sample taken from the warehouse bulk cement cylindrical, sampling is only done from one hole expenditures alone. When amount of bulk cement in storage exceeds 1200 tons, and if rectangular warehouse, cement samples taken but not out of the hole expenditure, such that the amount should represent more than half amount of cement stored in the warehouse. At the time cement is flowing through the hole expenditure take semen samples at any given time interval, so it must represent more than half of cement stored in the warehouse. At the time cement is flowing through the hole expenditure take semen samples at any given time interval, so that the flow of 400 tons of cement each taken at least 2 examples of quotes from bin or silo. 2) From the warehouse bulk cement and bulk cement ships using tools sampling. If the depth of bulk cement to be sampled not exceed 2.1 meters, a semen sample can be obtained by using a sampling for bulk cement are shown in Figure 1. length between 1.5 m to 1.8 m and an outer diameter of approximately 35 mm, consisting of 2 pipe coated brass with a series of holes that can be opened and closed with the rotate the inner pipe. Shaped pointy end of the outer pipe so as to facilitate for penetration. Take for example the cement of the points spread evenly with depth Different cement being taken so that the whole would be represented. 3) From the bags of cement by using a sampling device in the bag. Stick the bag sampling apparatus as shown in Figure 2, the transverse through hole bags of cement. Then close the air hole with mother finger, then pull the tool. Take an example of a bag of cement for every 5 tons or multiples thereof.

Figure 1 Pipe cement sampling

Figure 2 Pipe cement makers in the packaging 4) From the delivery of bulk cement by train or truck. (1) Single Delivery If the delivery is done only by using a single carriage or a cement truck, which is continuously loaded and are derived from one source, take a semen sample that weighs 5 kg. If not continuously loaded and unknown sources, combine 5 or more parts cement samples from several different points to used as a test sample. (2) Delivery plural If the shipment consists of several railroad car or truck loaded cement from the same source and the same day, take cement sample for every 100 tons or multiples thereof, but shall not be less from 2 examples. Treatment cement sample as an example of lots of cement. And test samples according to the procedures described in the "weight of sample for testing "

6.7 Storage cement sample After the cement sample is taken, immediately place it in a airtight and vapor water to prevent absorption of water or aeration of the cement sample. If the cement sample is placed in a place that is made of tin, cover tightly and immediately sealed. Use the bag consisting of several layers of impermeable paper water vapor, or a plastic bag, which was strong enough not to break, try immediately sealed after filling so that the air inside the bag out and moisture absorption and aeration prevented. Cement sample should be treated as described in the section "Preparation of sample test ". 6.8 Preparation of test sample Prior to testing, cement sifted through the sieve size 850 m (sieve no. 200 or other sieve size of openings that have roughly the same). In order to sample well mixed, divide the clumps, and grab dirt. Remove dirt and hardened clumps that can not be broken during sieving. Store airtight cement in place to prevent the absorption of steam water prior to the test 6.9 Failure to meet the requirements and retest 6.9.1 If any of the test results fail to meet the requirements, lot cement not reported as a cement that does not meet the requirements of the specification to failure to be confirmed by the number of retesting. 6.9.2 A retesting may comprise one type of test or the entire test fully. 6.9.3 Retesting should be done in accordance with the specifications used. If this provision is not given, the following procedure should be used. 6.9.4 Perform retesting of some examples of the cement used in the initial testing. Use other methods for the determination of the properties of cement required retesting and in this case only the test results obtained with other methods used. Retesting shall consist of a number of necessary determination as to initial testing. The number of repetitions used is fundamental to the provision accuracy. If two or more fixing is required, the price reported shall is the average price of all the test results that are at the limits of accuracy the method 95% confidence level, as stated in the specification used or known in general. 7 How to test 7.1 Chemical test methods Test methods include chemical analysis of hydraulic cement refers to ASTM C 114-03, Test Methods for Chemical Analysis of Hydraulic Cement. Each test method shows accuracy and acceptable deviation can be used for semen analysis hydraulics, including the referee test method, as described in paragraph 7.1.1 Specific chemical test methods provided for convenience for those who want to use it. The test method is classified as referee test method and

alternative test methods. The test method referee is wet chemistry test methods that have been received, which provide an integrated basic scheme of analysis of hydraulic cement. Alternative test methods generally provide individual determination of specific components and can be used alone or as an integrated alternative and determination when desired by the analyst as shown in the individual methods. Each analyst must be able to demonstrate high skill as described in paragraph 7.1.1, if this method is used. 7.1.1 Test methods of cement and variations are allowed 7.1.1.1 Referee test method Referee test methods such as listed in point 7.1.3.1 through 7.1.3.16 or other test methods established under clause 7.1.4, is used when the results of the analysis questionable referee test method meets the requirements of the chemical. In such cases, the cement can not be rejected because it does not meet the chemical requirements determination unless all the elements and all the preliminary separation have been taken by the referee test method. In case of doubt, the analysis should be done twice on different days. If the results are not in accordance with the permitted variation in Table 1, the determination repeated until 2 or 3 results meet variations allowed for purposes comparative analysis and calculation of average acceptable results, the percentage should be calculated to be as close to 0.01 (or 0.0001 for organic compounds that are soluble in chloroform), although there are some average results are reported to the accuracy of 0.1. Table 6 The difference in test results allowed difference No. Component maximum two testing 1. 2. 3. 4. 5. 6. 7. 8. 9. SiO2 (Silikon dioksida) Al2O3 (Aluminium oksida) Fe2O3 (Besi(III) oksida) CaO (Kalsium oksida) MgO (Magnesium oksida) SO3 (Sulfur trioksida) HP Na2O (Natrium oksida) K2O (Kalium oksida) 0,16 0,20 0,10 0,20 0,16 0,10 0,10 0,03 0,03 Maximum difference of The average twodetermination by SRM Certificate (unit in%) 0,2 0,2 0,10 0,30 0,2 0,1 0,10 0,05 0,05

10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

TiO2 (Titanium dioksida) P2O5 (Posfor pentaoksida) ZnO (Seng oksida) Mn2O3 (Mangan oksida) S (Sulfida) Cl (Klorida) IRInsoluble part FLCalcium oxide-free Sol ALK (Alkali-soluble in water CHL sol (organic compounds soluble in chloroform) 7.1.1.2 Alternative test methods

0,02 0,03 0,03 0,03 0,01 0,02 0,10 0,20 0,75/w 0,004

0,03 0,03 0,03 0,03 -

In some cases alternative methods provide procedures shorter or longer suitable for routine determination of certain components rather than the test method referee (NOTE 1). In some cases, the procedure is more complex and longer, still used as Alternative test methods to compare the results with different procedures or to be used if the specific material being tested with disorders that can suspected, or if the special preparation required for analysis. The test results from a test method alternatives may be used as a basis for acceptance or rejection if the results clearly showed that the cement actually meet or do not meet the requirements specifications. NOTE 1 It is not intended to limit the referee test methods for reference analysis. A referee test method be used instead of an alternative test method if so required. A reference test method should be used if no alternative test methods given. Analysis of double and blank determination is not required if using the test method alternatives. But if you want a blank determination for an alternative test, which is may be used and it is not necessary if already obtained simultaneously with analyzes. The end result, if corrected for blank values, in each case must be shown. 7.1.2 General 1) Reagents weight expressed as "approximately 5 grams of" reasonably weighted raw score. 2) Fill the solution represented by "approximately 300 mL fairly observed with the eye, fill the "10 mL" enough to fill

a measuring cup and declared "exactly 25 mL" should measured with a burette or pipette. 3) "Sale" shall mean the room temperature, "warm" temperature range (30-40) oC, and "hot" have interpreted the temperature close to the temperature of boiling water (90-95) oC. 4) Pembacan buret to 0.01 mL should be used and if it is a solution with a titer low, should be used micro burette. 5) When used in testing the water, the water is distilled water is aquades. 7.1.2.1 Equipment and materials 1Equipment 1Equipment scales: Scales analytic capacity of not more than 200 grams. Scales should be able to generate the readback the difference is not more than 0.0002 gram to the nearest 0.0002 gram. 2Laboratory equipment made of glass and polyethylene materials: a. Pumpkin peck, burettes and pipettes should be in a high degree of precision. b. Tools such as a special type of glass colored glass, high silica glass and alkali resistant glass. c. Containers made of polyethylene for all alkali solution and the solution standard. d. Desiccator equipped with hair such as magnesium perchlorate, activated alumina, or sulfuric acid. Anhydrous calcium sulfate may also used, but calcium chloride is not appropriate in this analysis. e. Filter paper: porous coarse, fine porous and porous medium. f. Krusibel: Krusibel made of platinum with a capacity (15-30) mL. g. Furnace: furnace is equipped with a precision pyrometers 25 oC. 2Materials For all test reagents should be used "chemical grade", unless advised other. Other reagents used must have a high enough purity without reducing the accuracy of the determination. 1The concentration of reactants a. Reagent ready to use Standard solution or a ready-made reagent concentrations have diluted it can be used when equipped specification of the level of purity. b. Concentrated acid and ammonium hydroxide When acids and ammonium hydroxide only equipped with requirements based on the name and chemical formula, it must be understood that should be in a state of concentrated reagent according to the Specific Gravity (SG) or concentration by weight as follows:

Acetic acidCH3COOH99.95 hydrochloric acidHCl1.19 b.j hydrofluoric acidHF48 nitric acidHNO31.42 b.j phosphoric acidH3PO485 sulfuric acidH2SO41.84 b.j Amonium hidroksidaNH 4 OH0.90 b.j

c. Acid and ammonium hydroxide solution Specified as a ratio of the volume of concentrated reagent the volume of water is added, for example, HCl (1 +99), meaning 1 volume of concentrated HCl (SG 1.19) was added to 99 volumes of water. d. standard solution The concentration of the standard solution is expressed in normality (N) or as equality in grams per milliliter of the specified component. At least three times a determination must be determined to get results average of standardization. e. Concentration of non-standard solution is prepared by dissolving the solid reagent in units of a certain weight that is dissolved in the solvent water, unless otherwise solvent. (2Indicator solution a. Methyl red: 2 grams of methyl red / L in 95% ethanol. b. Phenolphtalein: 1 gram phenolphthalein / L in 95% ethanol. 7.1.2.2 Sequence analysis of the reports of the chemical components of portland cement suggested. 1major components (1) SiO2 (Silicon dioxide) (2) Al2O3 (Aluminium oxide) (3) Fe2O3 (Iron (III) oxide) (4) CaO (Calcium Oxide) (5) MgO (Magnesium oxide) (6) SO3 (sulfur trioxide) (7) Missing incandescent

2minor component (1) Na2O (sodium oxide) (2) K2O (potassium oxide) (3) TiO2 (Titanium dioxide) (4) P2O5 (Phosphorus pentaoksida) (5) ZnO (zinc oxide) (6) Sulfide sulfur (7) Mn2O3 (Manganese Oxide) 3Separate Determination (1) Section insoluble (2) The organic compound is soluble in chloroform (3) Calcium oxide-free (4) Alkali-soluble in water

7.1.3 Methods referee 7.1.3.1 Section of insoluble 1Summary of test method In this method, the insoluble part of the semen sample was determined by mendigest in HCl. After filtering, the next didigest with sodium hydroxide. The residue obtained dipijarkan and weighed. If the test method is used to mix cement (blended cement), the decomposition the acid is considered perfect if slag Portland cement entirely biodegradable. Solution of ammonium nitrate used in the final washing to prevent the material is not soluble subtle escape from the filter paper. 2Reagents Solution of ammonium nitrate (NH4NO3 20 g / L). Solution of sodium hydroxide (NaOH 10 g / L). 3procedure (1) Weigh 1 gram of sample, insert it into the 250 mL beaker, add 25 mL of water and 5 ml of HCl. (2) If necessary, reheat the solution and tap-tap example with rod ends glass stirrer to unravel perfect. (3) Dilute the solution to 50 mL with hot water and heat in the hot plate to near boiling point. (4) Filter through a filter paper into a porous medium in 400-ml beaker, wash beaker, filter paper and precipitate 10

times with hot water and filtrate used for the determination of SO3. (5) Remove the filter paper and precipitate to the original beaker, add 100 mL hot NaOH solution (10 g / L) and didigest for 15 min at temperature almost boiling. (6) During didigest occasionally stir the mixture and mash filter paper with a stirring bar. Acidify with HCl solution and the use of methyl red as an indicator, add excess HCl (4-5) drops. (7) Filter porous medium with filter paper and wash the precipitate at least 14 times the heat NH4NO3 solution (20 g / L) to ensure that the filter paper and washed it perfectly. Filter paper and its contents krusibel put in a known weight. Fuel and pijarkan temperature (900-1000) oC for at least 30 minutes. chill in desiccator and then weigh it. (8) blank Perform a blank determination using the same reagents and yag way. Calculate the results as a correction in the calculation. 4calculation Calculate levels of insoluble parts with accuracy to 0.01% % insoluble part = heavy sediment heavy sample 7.1.3.2 Silicon dioxide (SiO2) For portland cement dissolution unknown part, first determine appropriate with clause 7.1.3.1. For portland cement part and wore a percentage less than 1%, continue to clause 7.1.3.2.1), to cement dissolution part greater than 1%, proceed to item (7.1.3.2.2). 1Silicon dioxide insoluble parts less than 1% (1) Summary of test method In this test method is silicon dioxide (SiO2) was determined by gravimetry. Add ammonium chloride and the solution should not be evaporated to dryness. This method was developed primarily for hydraulic cement that nearly unraveled perfect with hydrochloric acid and should not be used for hydraulic cement contains most of the ingredients are not soluble in acid and Sodium carbonate fusion requires first. To cement that way, or if you require a standard specification for cement analysis, procedure in point 7.1.3.2.2) should be used. 2Reagents Ammonium chloride (NH4Cl). X 100

Hydrochloric acid (HCl). Hydrochloric acid (HCl) (1 +99). Nitric acid (HNO3). Sulfuric acid (H2SO4) (1 +1). Hydrofluoric acid (HF). 3procedure 1) Mix the cement evenly 0.5 gram sample with approximately 0.5 g NH4Cl in 50 mL beaker, cover the beaker with watch glass and carefully add 5 ml of HCl with the pouring through the edge of the beaker. After the chemical reaction finished, take a watch glass, add 1 or 2 drops of HNO3, stirring mixed with glass rods, glass lid and place it back chemicals in the steam bath for 30 minutes. During the time this digest occasionally stir the contents of the glass and break the clumps which still exists to facilitate the decomposition Perfect from the cement. Attach a porous medium filter paper in a funnel, transfer silicic acid blob into the filter as much as possible without dilution, and let the solution drip. Scrub the wall of the beaker with a stirring rod fitted rubber polisher, and rinse the beaker and stir bar with hot HCl (1 +99). Wash the filter paper with hot HCl (1 +99) and then washing with water heat little by little as 10 or 12 times, save the filtrate and water laundry for grouping ammonium hydroxide 2Transfer the filter paper and precipitate into krusibel have known weight, dry and pijarkan slowly at temperatures low up carbon from the filter paper without any flame disappeared from the paper filter, then continue pemijaran temperature (1100-1200) C for 1 hour. Then pijarkan return to fixed weight (w1). Treat the SiO2 obtained which still contain slight impurities in krusibel with 1 mL or 2 mL of water, 2 drops of H2SO4 (1 +1) and approximately 10 mL HF, and uapkan carefully to dry. Finally pijarkan a little residue on the temperature (1050-1100) C for 5 minutes, cool in a desiccator and weigh (w2). The difference in weight between (w2) is given with prior HF (w1) is the weight of SiO2. Need remember heavy residue remaining after evaporation of SiO2 is a combination Aluminium oxide and iron (III) oxide, and enter into the solution obtained for determination of ammonium hydroxide groups.

3If the result of the evaporation of the HF exceed 0.0020 gram, determination silica should be repeated, steps should be taken to ensure the decomposition of the sample before the separation of silica done and subsequent determination of (Al2O3 + Fe2O3, CaO and MgO) are set with the new filtrate and the residue obtained after addition HF has a weight of 0.0020 grams or less, except as specified in paragraph 7.1.3.2.1.) (3) .4) and 7.1.3.2.1). (3) .5)

4If after two or three repeated determination and found that residues obtained after addition of HF remains greater than 0.0020 grams, then contamination may otherwise occur during sampling or during the cement manufacturing process is not firing perfectly. In such cases the sediment results are not be melted and added to the filtrate for the determination of class ammonium hydroxide, but report results as a result of sediment obtained. 5In these circumstances add 0.5 grams of sodium or potassium pirosulfat (Na2S2O7 or K2S2O7) into krusibel and heat almost incandescent to precipitate impurities dissolved, cool and dissolved in water and combine with the filtrate, and combine with the laundry kept for determination of ammonium hydroxide groups. 6Perform a blank determination using the reagents and test methods the same result as a correction into account in the calculation. 4Calculation Calculate the content of SiO2 with accuracy to 0.1%.

with: w1 is the weight of sediment before plus HF, g; w2 is the weight of sediment after the addition of HF, g; w is the weight of sample, grams. 2Silicon dioxide insoluble parts greater than 1% (1) Summary of test method The test method is based on the fusion of sodium carbonate followed by repeated evaporation of hydrochloric acid solution to dryness to change shape silica to form insoluble. The solution was filtered and precipitated silica insoluble dipijarkan and weighed. SiO2 evaporated with HF, then dipijarkan and weighed. (2Reagents Sodium carbonate (Na2CO3). Hydrochloric acid (HCl). Hydrochloric acid (HCl) (1 +3). Hydrochloric acid (HCl) (1 +99). Hydrochloric acid (HCl) (1 +1).

3procedure 1) Weigh a number of examples that have dipijarkan equivalent to 0.5 gram sample as calculated in accordance with the following formula:

W is the weight dipijarkan example, gram; HP is missing bulbs,%. Materials that have been lost dipijarkan the determination can be used as examples. Mix evenly with examples (4-6) grams of Na2CO3 to the road grinding in the agate mortar. Cover with a thin layer of base krusibel Na2CO3, add the mixture cement-Na2CO3 mixture on top then cover with a thin layer Na2CO3. Put krusibel who has covered over a medium flame and flame slowly increased to a maximum ( 1100 C) and maintain this temperature until the mixture quiscent ( 45 minutes). Move burner, open the place in other places, flops krusibel with clamp and swivel krusibel slowly so that the content in the form of spread melted and solidified as a thin layer on the inside walls of the cup. Refrigerate krusibel its lid. Rinse the wall next Outside of krusibel and place in a casserole with krusibel the third volume of 300 mL volume of water. Warm the casserole and stir so that the crust in the cracked krusibel and can be moved easily. By using a glass rod, remove krusibel of casserole, rinse with water until clean. Rinse krusibel and lid with HCl (1 +3), the rinse water is added to the casserole. Add 20 ml of HCl (SG 1.19) carefully and slowly to in a closed casserole. Remove and rinse the cover. if there are granular particles means imperfect smelting and testing should be repeated using a new instance. attention: The sequence of testing steps should be followed correctly to produce precise and accurate results. 2Evaporation solution to dryness on the steam bath (until no visible WISP) without further heating the residue, add (5-10) mL HCl, let stand at least 2 minutes, add the number of the same water (5 mL -10 mL). Close krusibel and digest for 10 minutes on the steam bath or plate heat. Dilute the solution with hot water by the same amount, porous filter medium with filter paper and wash separate SiO2 with hot HCl (1 +99), and then with hot water, keep sediment. 3Evaporation more filtrate to dryness and bake in the oven at deposition temperature (105-110) C for 1 hour, cooled, added (10-15) mL HCl (1 +1) and digest on a steam bath or hot plate for 10 minutes.

Dilute with the same amount of water, immediately filtered with paper new filter, and wash with SiO2 as in point 7.1.3.2.2.) (3) .2), stir filtrate mixed with water washing and save for grouping ammonium hydroxide in accordance with clause 7.1.3.3 grouping ammonium hydroxide. Continue SiO2 determination in accordance with clause 7.1.3.2.1.) (3) .2), remove the filter paper. 7.1.3.3 Group ammonium hydroxide (R2O3) 1Summary of test method In this method, aluminum oxide, iron (III) oxide, titanium dioxide, and phosphorus pentaoksida precipitated from the filtrate, after SiO2 separated by the addition of ammonium hydroxide. When done with more caution precipitated manganese dioxide will precipitate. Deposition dipijarkan and weighed as oxide. 2reagents Hydrochloric acid (HCl SG 1.19). Hydrochloric acid (HCl) (1 +2). Ammonium hydroxide (NH4OH) (1 +1). Ammonium nitrate (NH4NO3). 3procedure (1) The filtrate is stored in point 7.1.3.2.1.) (3) .1) (see item procedures) volume 200 mL, if necessary plus HCl to ensure the amount of acid entirely in the filtrate (10-15) mL. Add a few drops of methyl red indicator and heat up boil. Then drops NH4OH (1 +1) to yellow solution, and add one drop of excess. Heat the solution containing the precipitate to boiling and boil during (50-60) seconds. To avoid bumping during boiling solution it can done in other ways, namely: Men-digest on the hot plate having a temperature equal to the bath Steam for 10 minutes Let the sediment down (no more than five minutes) and filtered with a using porous filter paper medium. Wash with a solution of ammonium Hot nitrate (NH4NO3 20 g / L), for a slightly washed precipitate as twice, while for a lot of sediment washed four times. 2Collect the filtrate and precipitate its move into the paper screenprint beaker which was originally used for the deposition. Dissolve the precipitate with hot HCl (1 +2). Stir until the filter paper was destroyed and then dilute the solution to 100 mL of boiling water. endapkan back hydroxide corresponding point 7.1.3.3.3) .1). Filter the solution and wash the precipitate with (4-10) mL of hot ammonium nitrate (NH4NO3 20 g / L). Combine the filtrate and its solution pencucinya with original fitrat and save appropriate for the determination of CaO grains 7.1.3.9.3) .1).

3Place sediment in krusibel a known weight, heat slowly until the carbon from the filter paper is gone, and the last to prevent reduction, careful pijarkan temperatures (1050-1100) oC to severe fixed and weigh as ammonium hydroxide group. 4Perform a blank determination using reagents and a same result as a correction into account in the calculation. 4Calculation Calculate R2O3 levels with accuracy of 0.1% %R2O3 = heavy sediment heavy sample X 100

7.1.3.4 Iron (III) oxide (Fe2O3) 1Summary of test method Levels of cement Fe2O3 set of individual examples with reduction of iron (III) to iron (II) and tin (II) chloride (SnCl2) and titrated with a standard solution potassium bichromate (K2Cr2O7) This determination is not affected by the titanium and vanadium which may exist in cement. 2reagents (1) diphenilamine barium sulfonate indicator solution. Dissolve 0.3 grams of barium sulfonate diphenilamine in 100 mL of water (2) standard solution of potassium dichromate (1 mL = 0.004 g Fe2O3) Puree and dry reagents primary standard potassium dichromate (K2Cr2O7) NBS 136 at a temperature of (180-200) C until the weight remains. Weight carefully as 2.45700 grams to 1 liter of solution prepared. Dissolve in water and dilute to the right until the desired volume the right-sized pumpkin. This standard solution is a solution of a primary standard and do not need to be set again. (3) A solution of tin (II) chloride Dissolve 5 grams of lead (II) chloride (SnCl2.2H2O) in 10 ml of HCl and dilute to 100 mL. Add grains lead free iron and simmer until the solution in a bottle drops containing granules covered tin.

3procedure For part portland cement dissolution is not known, the first specify the portion insoluble in accordance with the test method described in this procedure. If the dissolution unknown part, take it as item 7.1.3.4.3). (1) or 7.1.3.4.3.) (2).

(1) For portland cement with high levels of insoluble parts less than 1%, weight 1 g sample into a 500 mL beaker or other suitable container. Add 40 mL of cold water, while the container shaken add 10 ml of HCl. If you need to reheat the solution and break cement with rod led flat glass until all the cement breaks down perfectly. Continue analysis corresponding point 7.1.3.4.3). (2). a). (2) For cement with high levels of insoluble parts greater than 1%, weight 0.500 grams of sample, mixed with 1 g LiBO2 using mortar and pestle. Move into a pre-heated krusibel containing 0.1 grams LiBO2 scattered at the bottom. Close to 0.1 grams LiBO2 is first used to clean the mortar and pestle. Place the lid on the stove did not krusibel the temperature is set at 1100 C for 15 minutes. Move krusibel from the smelting furnace and check perfection. If the melt is not perfect, krusibel back into the furnace for 30 minutes. Check back melting perfection. If fusion remains incomplete, exhaust sample and repeat the procedure using a 0.250 gram sample melting or number fewer instances with the same number of LiBO2. If the melt is complete, immediately shake, carefully melt and pour into a 150 ml beaker containing 10 ml of HCl and 50 mL of water. stirring constantly fused again until late results, usually 10 minutes or less. If you use a magnetic stirrer, remove and rinse the stirring rod and continue the analysis of corresponding point 7.1.3.4.3). (2).a). a) Heat the solution to boiling and add drops of SnCl2 solution by drop while stirring and boiling until the solution is colorless. Add one drop of excess and cool the solution to room temperature by placing the beaker in a pan of cold water. After the cold and without delay rinse the inside of the glass wall chemically with water, and add 10 mL of saturated as well as mercury chloride (HgCl2) cold. Stir the solution rapidly for one minute in a way shake the beaker and add 10 mL H3PO4 (1 +1) and two drops of indicator solution diphenilamine barium sulfonate. Add water sufficiently to volume after titration ranged between (75 -100) mL. Titration with a standard solution of potassium dichromate. The end point is indicated where one drop causes the red color violet fixed to the addition of excess K2Cr2O7 solution. 4blank Perform a blank determination using the procedures reagents same. Record volume of K2Cr2O7 solution required to establish endpoint as described in paragraph 7.1.3.4.3.) (2). a). Required amount of iron that reaches the end point, if the color is not visible amber clear after the addition of four drops of the K2Cr2O7 standard solution the blank contained no iron. 5Calculation Calculate the content of Fe2O3 with 0.01% accuracy (reported to the nearest 0.1%) as follows:

with: E is equal to the solution of K2Cr2O7 Fe2O3, g / mL; V is milliliters of K2Cr2O7 required in setting an example; B is milliliters of K2Cr2O7 required on blank determination; W is the weight of sample to the nearest 0.1 milligram. 7.1.3.5 Pentaoksida Phosphorus (P2O5) 1Summary of test method Colorimetric assay method is used to determine P2O5 in portland cement. In the test condition is usually no other element that may interfere in portland cement. 2Equipment Spectrophotometer Instruments must be equipped to measure the absorbance of the solution in the long wave 725 nm. Wave length measurements should be repeated within a tolerance of 1 nm or smaller. In the area of absorbance of 0.1 to 1.0, absorbance measurements must be repeated in tolerance of 1% or less. To ensure that the spectrophotometer can be used with a level of accuracy satisfactory, qualified in accordance with the specifications of the instrument using procedure 7.1.3.5.4). 3Reagents (1) A solution of ammonium molybdate Enter 10.6 N 500.0 mL H2SO4 in 1 liter measuring flask Dissolve 25.0 grams of ammonium molybdate (NH4) 6Mo7O24.4H2O) in 250 ml of warm water and transfer to a measuring flask containing H2SO4, while shaken flask. Cool, dilute to 1 liter with water, and store in a plastic bottle. (2) Ascorbic acid powder To facilitate dissolution, using the most refined. 3Standard hydrochloric acid (6.5 0.1 N) Dilute 540 ml of HCl (SG 1.19) to 1 liter with water. Standardise against standard NaOH solution 7.1.3.5.3). (6) by using phenolphthalein indicator. Determine the exact normality and set in 6.5 N 0.1 N with dilution water. Standardise normality back to ensure that the right has been reached. (4) A phosphate standard solution

Dissolve 0.1917 g of potassium dihydrogen phosphate (KH2PO4) that has been dried to in water and dilute to 1 liter in a measuring flask. 5Phosphate standard solution B Dilute 50 mL of phosphate solution A to 500 ml with water. (6) standard solution of sodium hydroxide (1 N) Dissolve 40.0 grams of sodium hydroxide (NaOH) in water, add 10 mL solution of saturated solution of barium hydroxide (Ba (OH) 2) The new filtered, and Dilute to 1 liter with water that has just boiled and cooled. Shake the solution from time to time for a few hours, and strain into a plastic bottles. Keep bottle tightly closed to protect the solution of the CO2 in the air. Standardise against phtalat potassium acid or benzoic acid in acidimetry issued by NBS (standard sample 84 f and 350), with using the test methods in the certificate accompanying examples. Set the appropriate solution normality. (7) Standard sulfuric acid (10.6 N 0.1 N) Into a 1-liter flask cooled in water, add more or less 600 mL of water, then add 300 mL of H2SO4 (bj 1.840) with a gradual and carefully. After cooling to room temperature, dilute to 1 liter with water. Standardise against standard NaOH solution 7.1.3.5.3). (6). using phenolphthalein as an indicator. Set normality and set to 10.6 N 0.1 N with dilution water. Standardise normality back to ensure that the right has been reached. 4) Procedures (1) Prepare a series of phosphate solution (0 -0.5)% P2O5 Prepare each by adding the appropriate volume of solution B raw phosphate and 25.0 mL 6.5 N hydrochloric acid in 250 mL measuring flask. (NOTE 2). Dilute with water to mark boundaries. NOTE 2 One milliliter of phosphate standard solution B in 250 mL of solution equivalent to 0.004% P2O5 gram sample of cement. A list of the concentrated solution (mother liquor) the volume of raw phosphate B: 0; 12.5, 25, 50; 74; 100 and 125 mL equivalent P2O5 levels in semen samples at 0; 0.05; 0.10, 0.20; 0.30; 0.40, and 0.50%. (2) Prepare a blank by adding 25.0 mL of HCl into the flask pint of raw 250 mL and dilute to 250 mL with water. Perform staining on Phosphate solution and blank rows in accordance with Section 7.1.3.5.4). (5) to 7.1.3.5.4). (7) so that the resulting color. (3) Plot absorbance values (raw absorbance minus blank absorbance) obtained as P2O5 concentration as ordinate and abscissa. Create curves shows the relationship between the absorbance against the concentration of P2O5.

(4) Move the 0.25 grams of sample into a 250 mL beaker and wet with 10 mL of cold water to prevent clumping. Add 25.0 mL of HCL raw and digest with the help of heating medium and stirred until the solution is perfect. Filter into a 250 mL measuring flask and wash the filter paper and precipitate silica Separate with hot water. Let the solution cool and dilute with water up to 250 mL. (5) Transfer 50.0 mL aliquot of sample into a 250 mL beaker, add 5.0 mL of a solution of ammonium molybdate and 0.1 grams of ascorbic acid powder. Stir the contents of the beaker shaken up by ascorbic acid dissolved perfectly. Heat the solution to boiling, remove the cover and continue boiling during (1.5 0.5) minutes. Cool to room temperature and move into 50 mL measuring flask. Rinse the beaker with a little water and add the rinse water into a measuring flask. Dilute to 50 mL with water. (6) Perform a blank measurement at a wave length of 725.0 nm. (7) Prepare a 50.0 mL aliquot prepared blank solution as the solution examples. Measure absorbance in accordance with Section 7.1.3.5.4). (6) and subtract the value absorbance obtained for the sample solution in items to 7.1.3.5.4). (5).In order to obtain the final absorbance of the sample solution. (8) Using pure absorbance values obtained, record the percentage P2O5 in the semen sample as shown in the calibration curve. Report to the nearest 0.01% P2O5.

7.1.3.6 Titanium dioxide (TiO2) 1) Summary of test method In this test method is titanium dioxide (TiO2) in the specified portland cement Tiron using colorimetric reagents. In testing conditions, only iron an element in portland cement which causes very little disruption, equivalent to 0.01% for every 1% Fe2O3. 2) Equipment spectrophotometer Instruments must be equipped to measure the absorbance of the solution in the long wave 410 nm. Wave length measurements should be repeated if obtained 1 nm. In the area of absorbance of 0.1 to 1.0, absorbance measurements must be repeated in tolerance of 1% or less. 3) Reagent (1) Buffer pH 4.7 68 g NaC2H3O2.3H2O plus 380 mL water and 100 mL of 5 N CH3COOH

(2) disodium salt dihydrate etilendinitro tetra acetic acid (EDTA 0.2 M) Dissolve 37.5 g EDTA in 350 ml of warm water and filtered Add 0.25 grams FeCl3.6H2O and dilute to 500 mL. (3) Hydrochloric acid (1 +6) (4) standard hydrochloric acid (6.5 N) Dilute 540 ml of HCl (SG 1.19) to 1 liter with water. (5) Ammonium hydroxide (NH4OH) (1 +1) (6) Potassium pirosulfat (7) Titanium dioxide, the mother liquor A Melting slowly 0.0314 gram 99.74% TiO2 (NBS SRM 154b) in krusibel over a small flame or other titan compound as a substitute and add approximately 2 g or 3 g K2S2O7. Let stand until cool, and krusibel in a beaker containing 125 mL of H2SO4 (1 +1). Heat and stir until melted completely dissolved. Cool, transfer to a 250 mL measuring flask, and dilute the solution to limit sign. (8) Titanium dioxide, aqueous standard solution B (1 mL = 0.0125 mgram TiO2) Pipet 50 mL of mother liquor A TiO2 into 500 mL 500 mL measuring flask, and Dilute to mark boundaries. One mL is equal to 0.0125 mg TiO2 which is equivalent to 0.05% TiO2 when used procedure in point 7.1.3.6.4). (5) up to the point 7.1.3.6.4). (6) (9) Sulfuric acid (1 +1) (10) Tiron (disodium-1 ,2-dihidroksidabenzen-3, 5 disulfonic acid) 4) Procedures (1) Prepare a series of aqueous standard solutions covering the concentration of B TiO2 0% -1.0% TiO2. Prepare each solution in a 50 mL measuring flask. NOTE 3 B mL standard solution diluted in 50 mL TiO2 which is equivalent to 0.05% to 0.2500 gram sample TiO2 semen.Larutan 0, 5, 10, 15 and 20 mL of solution equivalent to the raw TiO2, TiO2 content in the sample 0; 0.25; 0.50; 0.75, and 1%. (2) Dilute each to 25 mL with water. Add chemical reagent in accordance with the procedures in paragraph 7.1.3.6.4.) (5) to arise colors. (3) Measure absorbance in accordance with Section 7.1.3.6.4). (6) (4) Plot the value of absorbance as ordinate and the concentration of TiO2 as abscissa. For curve showing the relationship between the absorbance against concentration. (5) Transfer 25.0 mL aliquot of sample prepared in point 7.1.3.6.4.) (4) (see determination of P2O5) in a 50 mL

measuring flask. Add 5 mL and 5 mL EDTA Tiron, stir and then add drop by drop NH4OH (1 +1) Stirring is done carefully after each drop until there color change from yellow to green, blue, or red ruby. then return a yellow color by adding dropwise HCl (1 +6) and stir after each drop. Add 5 ml of buffer, dilute to mark boundaries and shake (6) Measure the absorbance of blank solution at a wavelength of 410 nm (7) By using absorbant prices specified in paragraph 7.1.3.6.4.) (6), record levels of TiO2 semen samples as shown in the calibration curve to the nearest 0.01. Correction of the iron in the sample to determine the actual TiO2 the following formula: Actual =% TiO2 TiO2 measurement - (0.01 x% Fe2O3). Report to the nearest 0.01% TiO2. 7.1.3.7 zinc oxide Each test method can be used in the testing of zinc oxide, provided able meet appropriate persyaratn differences listed in the table of test results is allowed (Table 6). 7.1.3.8 Aluminium oxide calculation: Calculate the percentage by reducing the amount of Al2O3 Fe2O3, TiO2 and P2O5 of percentage ammonium hydroxide groups. All fixing must referee methods such as described on the items in question. All percentages should be calculated to the nearest 0.01%. Report Al2O3 with 0.1% accuracy for the analysis of non referees, the percentage of Fe2O3, TiO2 and P2O5 can be determined with some qualification procedure has been demonstrated. 7.1.3.9 Calcium oxide (CaO) 1) Summary of test method In this test method, manganese removed from the filtrate after the determination of SiO2 and ammonium hydroxide groups. Then precipitated calcium oxide as oxalate. After filtration, redissolved oxalate and titration with potassium permanganate (KMnO4). NOTE 4 For referees or test methods for the determination with high accuracy, separation of manganese in accordance item 7.1.3.9.3). (2) For the determination of the low accuracy, and if only the amount of manganese oxide does not mean it is in point 7.1.3.9.3). (2) may be neglected. Strontium is usually found in portland cement as a minor element, and precipitated together with calcium as the oxalate and then titrated and calculated as CaO. If the levels are known SrO and CaO to SrO desired correction, for example, for research purposes or to compare the results with the certified values SRM, CaO determined by this

method may be corrected for SrO. In the determination to meet the specifications of cement, correction of CaO to SrO not should be done. 2reagents (1) A solution of ammonium acetate (50 g / L) (2) standard solution of potassium permanganate (0.18 N), prepare a solution of potassium permanganate (KMnO4) containing 5.69 g / L. Let this solution at room temperature for at least one week, or boiled and cooled to room temperature. Transfer the clear solution without disturbing the sediment on the bottom of the bottle; then filter the solution through a funnel had been separated a given glass wool pad or through a glass filter. Do not sift through material containing organic matter. Store in a dark bottle, preferably bottles that have been painted black on the outside. Standardise against (0.7000 to 0.8000) g of primary standard sodium oxalate, according with hints of standardization of sodium oxalate, and record the temperature at the time standardization is done (NOTE 5). Calculate CaO equivalence of the solution as follows: 1 ml of 1N KMnO4 solution is equivalent to 0.06701 grams of pure sodium oxalate. KMnO4 normality = Weight Na oxalate x fraction purity mL of KMnO4 x 0.06701 1 ml of 1N KMnO4 solution is equivalent to 0.02804 grams of CaO F = Normality solution of KMnO4 x 0,2804 x 100 0,5 with: F is equal to the solution of KMnO4 in CaO% CaO / mL based on a 0.5 gram sample of cement. NOTE 5 For KMnO4 solution is not stable, then the solution is re-standardized at least once every two months 3) Procedure (1) acidify the filtrate combined set on settling the ammonium hydroxide 7.1.3.3.3). (2). Neutralize with HCl until the color is methyl red end point, add Excess HCl 6 drops that really sour. (2) Separation of manganese Evaporation up to 100 mL volume Add 40 mL of saturated bromine water to a solution of the heat and immediately add NH4OH until the solution is alkaline. The addition of 10 mL NH4OH generally sufficient. A sheet of filter paper approximately an area of 1 cm2, put into a beaker and tap-tap it down with the rod tip to help prevent bumping and early deposition of manganese oxide hydrate (MnO). Boil the solution for 5 minutes or so, make sure the solution is

really alkaline any time. Let the sediment down, filtered using filter paper porous medium, and wash with hot water. If precipitation does not appear immediately, allow up to one hour settling time before the filter. Separate each manganese dioxide that has been settled. Acidify the filtrate with HCl using litmus paper as an indicator and boil until the bromine Evaporated (NOTE 6). (3) Add 5 mL HCl, dilute to 200 mL and add a few drops methyl red indicator and 30 ml of hot ammonium oxalate (50 g / L) (NOTE 7). Heat the solution to (70-80) oC and add NH4OH (1 +1) drop by drop, while stirring until the color changes from red to yellow (NOTE 8). Let the solution without further warming during (60 5) minutes (not more), with occasional stirring for 30 minutes. 4Filter uses fine filter paper, and wash the precipitate 8 to 10 times with hot water, the total amount of water used in rinsing beaker and washing should not exceed 75 mL. During this wash water from the wash bottles should directly lead to part the filter paper, to precipitate down, then spray with water slowly straight toward the center so that the filter paper sludge mixed and washes perfectly. Acidify the filtrate with HCl and stored for determination MgO. 5Place the beaker under the funnel containing the precipitate, cut peak filter paper cone with a stirring rod, place the rod in the beaker, and wash the precipitate into the beaker and wash sediment into the beaker with hot water. Squirt 10 drops of H2SO4 (1 +1) around the upper edge of the filter paper. Wash the filter paper with 5 times hot water. Dilute to 200 mL, and add 10 mL of H2SO4 (1 +1). Heat the solution at temperatures close to the boiling point, and immediately titrate with 0.18 N KMnO4 solution (NOTE 5). Continue titrating slowly until just pink color that persists at least 10 seconds. Add the filter paper containing the precipitate and soak. If the color pink does not appear, continue titration until the color is not at least for 10 seconds. NOTE 6 potassium iodide starch paper can be used to show perfection evaporation of excess bromine. Wear a damp paper on steam boiling solution. The paper should not change the color, and if the paper turns to blue means there bromine. NOTE 7 If a solution of ammonium oxalate is not clear, this solution should be filtered before use. NOTE 8 neutralization should be done slowly, otherwise, sediment calcium oxalate tends to pass through the filter paper. If a determination is made simultaneously following techniques can help to ensure neutralization slowly. Add 2 or 3

drops of NH4OH to the first beaker with stirring, then 2 or 3 drops into a second beaker, and so on, back to the first beaker with the addition of 2 or 3 drops again until the color of the indicator in the respective beaker changed. NOTE 9 temperature of 0.18 N KMnO4 solution as penetration can not be varied standardization of temperature more than 5.5 oC. Larger deviations can cause serious errors in the determination of CaO. 4blank Create a blank determination with the same procedure and using a number of The same reagent (NOTE 10) and record milliliters KMnO4 needed to endpoint determination. NOTE 10 When very small amounts of calcium oxalate, oxidation by KMnO4 running slow. Before titration MnSO4 add a little to the solution as a catalyst. 5calculation Calculate the percentage of CaO with precision 0.1 as follows:

with: E is equal to the solution of KMnO4 in CaO% CaO / mL based at 0.5 gram sample; V is a solution of KMnO4 required by the sample, mL; B is a solution of KMnO4 required by the blank, mL. If necessary, the correction percentage CaO to SrO as follows:

7.1.3.10 Magnesium oxide (MgO) 1) Summary of test method In this test method, magnesium precipitated as magnesium ammonium phosphate separated from the filtrate after calcium. Deposition dipijarkan and weighed as ammonium pyrophosphate (Mg2P2O7). Equality MgO is then calculated. 2) Reagent Ammonium phosphate dibasic (100 g / L) (NH4) 2HPO4. 3Procedure Acidify the filtrate from the determination of CaO 7.1.3.9.3). (4) with HCl and uapkan with boiling up to approximately 250 mL. Cool the solution to room temperature, add 10 ml of ammonium phosphate ((NH4) 2HPO4) dibasic (100 g / L) and 30 mL NH4OH. Stir the solution vigorously for the addition of NH4OH and then extend stirring time 10 minutes -15 minutes. Allow the solution for at least 8 hours on the air temperature. Wash residue 5 or

6 times with NH4OH (1 +20) and pijarkan in krusibel or porcelain cup of known weight, at first slowly heated until the filter paper into charcoal filter and then burn (NOTE 11), and pijarkan finally at 1100 C for 30 minutes - 45 minutes. Weigh the residue as magnesium pyrophosphate (Mg2P2O7). 4Blank Create a blank determination with the same procedure and using a number of The same reagents and correction results obtained in the analysis. 5) Calculation Calculate the percentage of MgO to the nearest 0.1 as follows:

with: W is a gram Mg2P2O7; 72.4 is the ratio of MgO to Mg2P2O7 molecule 2 (0.362) divided by weight examples used (0.5 grams) multiplied by 100. NOTE 11 The work must be done carefully during this pemijaran. Sediment phosphate can be reduced if the contact with carbon at high temperatures. There is a possibility of trapping harmful carbon deposition on the pemijaran which is too fast. 7.1.3.11 Sulfur 1) Sulfur trioxide (1) Summary of test method In this test method sulfate precipitated from acid solution of cement with barium chloride (BaCl2). Deposition dipijarkan and weighed as barium sulphate (BaSO4) and calculated SO3 equality. (2) Procedure At 1 gram sample, add 25 ml of cold water while stirring mixed firmly and add 5 mL of HCl (NOTE 13) If you need to heat and destroy the sample solution by the end of the rod flat glass stirrer ended up perfectly biodegradable cement (NOTE 14). Dilute the solution to 50 mL and digest for 15 minutes at a temperature of nearly boil. Filtered through a porous medium filter paper and wash the residue with hot water. Dilute the filtrate to 250 mL and heat until boiling. Add slowly dropwise 10 mL of hot BaCl2 (100 g / L) and continue boiling until the precipitate formed. Digest solution for (12-24) hours at a temperature of almost boiling (NOTE 15). Keep the volume of solution between (225-260) mL, and add water if necessary. Filter through fine porous filter paper, wash the precipitate with

hot water, put filter paper and its contents in a weighed krusibel. Pijarkan temperature (800-900) C, cooled in a desiccator and weigh. NOTE 12 When used with the instrument test method for sulfur or when comparing the results of the analysis of wet and instrument test method is less than 0.05%. NOTE 13 filtrate acid produced in the determination of insoluble residue 7.1.4.1.3) can be used for the determination of SO3 but to use another example. NOTE 14 brown residue of manganese component is negligible NOTE 15 When determining how quickly you want, a digest can be accelerated became the fastest 3 hours. Nevertheless cement may be rejected because it meets requirements specification, based only on the results obtained when using a digest (12-24) hours. 3blank Create a blank determination with the same procedure and use a number of The same reagents and correction results obtained in the analysis. (4) Calculation Calculate the percentage of SO3 to the nearest 0.01 as follows:

with: W is a gram BaSO4 for example; 34.3 is a comparison against BaSO4 molecules SO3 (0.343) multiplied by 100. 2) Sulfide (1) Summary of test method In this test method, sulphide sulfur determined by the gradual change as hydrogen sulfide (H2S) from the acid solution from the cement in solution ammoniakal zinc sulfate (ZnSO4) or cadnium ammoniakal chloride (CdCl2). Sulfide sulfur is titrated with a standard solution of potassium iodate (KIO3). Sulfite, thiosulfate and among other compounds sulfide and sulfate did not exist. If the compounds are included, can lead to errors in determination. (2) Equipment Pumpkin gas plant Connect the boiling flask 500 mL dry with a long-stemmed funnel separator through a rubber bulb cover. Separation funnel bent stalks arranged so not interfere with the bulb connector, separator funnel dipped end of the shaft get to the

bottom boiling flask, funnel connecting the separator to the compressor air. Connect the bulb with L shape glass pipe and glass pipe straight length 200 mm. Place the cup straight into the 400 mL beaker tall. pumpkin distillation three-necked with long gas tube placed between the compressor and separator funnel and into appropriate tools to regulate the air flow. Rubber used in this equipment must have a purity level high, with a low sulfur content and should be washed with warm HCl. (3) Reagent a. Solution of cadmium chloride amoniakal Dissolve 15 g of cadmium chloride (CdCl2.2H2O) in 150 mL of water and 350 mL NH4OH. b. Zinc sulfate solution ammoniakal Dissolve 50 grams of zinc sulfate (ZnSO4.7H2O) in 150 mL of water and 350 mL NH4OH. Filter the solution once it is left for at least 24 hours. c. Standard solution of potassium iodate (0.03 N) Prepare a solution of potassium iodate (KIO3) and potassium iodide (KI) as follows: Heat KIO3 at 180 C to constant weight. Balanced 1.0701 grams of KIO3 and 12 grams of KI. Dissolve and dilute to 1 liter in a measuring flask. Primary standard solution does not need to be standardized (NOTE 16) One milliliter of this solution is equivalent to 0.0004809 grams of sulfur. NOTE 16 This solution is very stable, but it must be standardized back every will use.Solution one year old should be discarded or concentration standardized return. d. A solution of tin (II) chloride Into a small flask containing 10 grams of tin (II) chloride (SnCl2.2H2O), add 7 ml of HCl (1 +1), warm the mixture gently to salt dissolved, cool the solution, and add 95 mL of water. This solution should be prepared in times of need, since this salt tend to be hydrolyzed. e. starch solution To 100 mL of boiling water, add cold suspension of 1 gram of starch solution in 5 mL of water and chill. Add a solution 1gram cold sodium hydroxide (NaOH) in 10 mL of water, then 3 grams of potassium iodide (KI), and stir vigorously. 4procedure Place 15 mL solution amoniakal ZnSO4 or CdCl2 solution ammoniakal (NOTE 18) and 10 mL of water into the flask,

and shake the wet and dispersed cement until it was perfect. This step and the addition of SnCl2 should be done quickly to prevent the binding cement. Connect the flask with a funnel and a bulb. Add 25 mL of SnCl2 through the funnel and the flask shaken. During the agitation, keep the funnel closed and drainage tube was in ZnSO4 solution ammoniakal or CdCl2 ammoniakal. Connect the funnel with a pressurized air source, open funnel, starting circulate air slowly to the boil. Continue boiling gently for 5 or 6 minutes. Stop heating and air jetting continue for 3 or 4 minutes. Remove the drainage tube and allow the solution to be used as mixer Cool the solution to a temperature (20-30) C (NOTE 19), add 2 mL starch solution and 40 ml of HCl (1 +1) and immediately titrate with 0.03 N KIO3 solution until the blue color that does not get lost again (NOTE 16). NOTE 17 In general ZnSO4 better than CdCl2 as ZnSO4 easy soluble in NH4OH from the CdCl2. CdCl2 solution can be used if doubt presence of trace amounts of sulphide sulfur, because of the yellow color of cadnium sulfide (CdS) can detect these trace amounts. NOTE 18 If the sulfur content exceeds 0.2 or 0.25%, to use an example a little so titration with a solution of KIO3 not exceed 25 mL. NOTE 19 Cooling is very important because different end points in the solution warm. NOTE 20 If the sulfur content is quite adequate but can not be predicted previously, the results obtained may be lower than it should be because loss of H2S during the slow titration. In this case, such determination shall repeated with the titration done faster. Perform a blank determination with the same procedure and using the reagents the same time, record the volume of KIO3 solution required to determine the end point as described in clause 7.1.3.11.2). (4). 5calculation Calculate the percentage of sulphide sulfur (see clause 7.1.3.11.2) as follows:

with: E is equal to the solution of KIO3 sulfide; V is KIO3 solution required by the sample, mL; B is KIO3 solution required by the blank, mL 20 = 100 divided by the weight of sample used (5 grams).

7.1.3.11 Missing incandescent 1Portland cement (1) Summary of test methods In this test method in cement dipijarkan furnace at temperatures set The missing part is assumed to indicate the amount of water and CO2 in the cement. This procedure is not appropriate to determine the lost glow of portland blast furnace slag cement and slag cement. (2) Procedure Weigh 1 gram of sample in a known weight krusibel. Cover and pijarkan krusibel its contents to constant weight in a heating furnace at a temperature of (950 50) oC. Allow at least 15 minutes for pre-heating time and at least 5 minutes for each subsequent time period. 3Calculation Calculate the percentage of missing bulbs with precision 0.1 by multiplying the weight lost in grams by 100.

with: W1 is the initial sample weight; W2 is the weight of the remaining sample bulb. 2Cement portland blast-furnace slag cement and slag (1) Summary of test method This test method provides correction weight gain due to oxidation of the sulphide is usually the case in portland cement blast-furnace slag and cement slag to determine SO3 levels rise during pemijaran. (2) Procedure a. Weigh 1 gram of sample in a platinum krusibel been fixed and pijarkan glow in the furnace and electric furnace at a temperature of (950 50) C for 15 minutes. Cool at room temperature in a desiccator and weigh. without should be constant, carefully move the material into the beaker 400 mL. Destroy clots in the cement with flat tipped rod. b. Determine the content of SO3 by methods 7.1.3.11.1). (1) to 7.1.3.11.1). (4). Specify the SO3 content of cement that are yet to be dipijarkan, the same procedure

3calculation Calculate the percentage of weight loss that occurs during heating and add 0.8 x SO3 Percentage difference from samples that had been heated and the original cement. Report the percentage that has been corrected as missing levels incandescent. 7.1.3.13.1 Sodium and potassium oxide 1alkali total 1) Summary of test method This test method covers the determination of sodium oxide (Na2O) and potassium oxide (K2O) the method of flame photometry or atomic absorption spectrophotometry method. NOTE 21 The test method is suitable for hydraulic cement that decomposes completely by HCl and should not be used for the determination of total alkali containing hydraulic cement material insoluble in high acid, such as cement Pozolan. But it can be used to determination of acid-soluble alkali course for cement. 2) Equipment All types of flame photometer or atomic absorption spectrophotometer can be used provided that the level of precision and accuracy in accordance with the specifications. NOTE 22 For routine testing in the laboratory, it is recommended checking the accuracy instrument done regularly anyway, either using standard cement NBS (National Bureau of Standards) or the alkali content of the cement is known. 3Reagents and materials (1) Containers laboratory All containers must be made of boron silicate glass and polyethylene containers must meet the requirements in accordance with Section 7.1.2.1.1). (2). (2) Calcium carbonate Calcium carbonate is used in the preparation of standard solution of calcium chloride may not have the total alkali as sulfate greater than 0.020% NOTE 23 The materials are sold as raw or primary ACS "low alkali" usually meet this requirement. However, the buyer should be sure that the material used really fit the requirements. (3) Calcium chloride (KCl) (4) Sodium chloride (NaCl)

(5) The solution in the market can be used instead of the solution in Below. 4preparation of the solution (1) The mother liquor of calcium chloride Add 300 mL of water into 112.5 grams of CaCO3 in 1500 beaker mL. While stirring, slowly add 500 mL HCl. Cool the solution up to room temperature, strain into a 1 liter measuring flask, dilute to 1 liter and perfect shake. The mother liquor is equivalent to 63,000 ppm (6.3%) CaO. (2) The mother liquor of sodium-potassium chloride Dissolve 1.8858 grams of sodium chloride (NaCl) and 1.583 grams of potassium chloride (KCl) in water (both dried at temperatures (105-110) OC for several hours before weighing). Dilute to 1 liter in a measuring flask and shake it perfectly. The mother liquor was equivalent to 1000 ppm (0.10%) respectively for Na2O and K2O. Separate solutions of Na2O and K2O can use home solution equally well to calibrate concentration and semen analysis. 3standard solution Prepare a standard solution necessary to instrument method used. Measure the required volume of mother liquor NaCl - KCl with using a dropper or pipette has been calibrated. The mother liquor of calcium chloride, if needed, can be measured with adequate measuring cup. If instruments used in the standard requires, measuring the standard solution with pipette or burette. Place each solution in the measuring flask, dilute to mark boundaries, and perfect shake. If necessary a more dilute solution in this method, the pipette solution necessary diluted into proper-sized pint flask, when necessary to add the standard solution, dilute to mark boundaries, and perfect shake. 5calibration In accordance with the manufacturer's operating instructions 6procedure (1) Solution cement Prepare a solution of cement in accordance with the special procedures of the manufacturer. If there is no special procedure, or if necessary, do in accordance with the specification clause 7.1.3.13.1.6) (1). (a) or 7.1.3.13.1.6). (1). (b).

NOTE 24 The presence of SiO2 in solution affect the accuracy of some tools flame photometer. In this case the instrument failed to yield to the level of accuracy is desired, the test should use his solution separated SiO2. Separation method in accordance with the method below. (a) Place (1.000 0.001) g of cement into a 150 mL beaker and dispersikan with 20 mL of water by shaking the beaker, while shaken add 5.0 mL of HCl once. Dilute immediately by up to 50 mL with water. Destroy clumps dispersed cements flat end of the rod. Digest on a steam bath or hot plate for 15 minutes, then strain porous medium with filter paper into a 100 mL measuring flask. Wash the beaker and paper with hot water, cool it to a temperature measuring flask space, dilute to 100 mL, shake the solution until it was perfect. b) Place (1.000 0.001) g of cement into the vaporizer cup platinum and dispersikan with 10 mL of water by shaking. She rocked, add 5.0 mL of HCl once. Destroy blob with a flat tip rod and heat on steam bath until dry. Make sure that the gelatin does not form again. Treat the residue with 2.5 mL HCl and approximately 20 mL of water. Digest on steam bath for 5 minutes - 10 minutes and immediately filtered through a filter paper 9 cm in diameter into 100 mL measuring flask. Perfect wash by washing repeated with a number of hot water until the total volume of the solution to 80 mL 95 mL. Cool to room temperature, dilute to mark boundaries, and shake it perfectly. When it was found that the separation of SiO2 is necessary to obtain accuracy the desired for a particular flame photometer, SiO2 should always be separated when analysis will be used as a basis for rejection because it does not meet the requirements, or doubt meet specifications. When you meet the specification, analysis was performed with this instrument without SiO2 separation, provided that deviations from price certificate obtained from testing is done, there should be two times greater than the limit indicated. c) If the test method requires the use of a more dilute solution, standard, or both, do the same dilution as the clause 7.1.3.13.1.4). (3). Standard solution and the sample solution to be analyzed must be prepared by the same and the same dilution as the solution of the cement analyzed for instrument qualification. 2Procedures for Na2O (NOTE 26) Heat and set the instrument for the determination of Na2O as described in clause 7.1.3.13.1.5). Promptly instrument settings, atomisasikan solution cement solution and record the scale reading (NOTE 25). Choose a solution distribution of raw Na2O levels approached the levels of Na2O in cement solution and do readings transmitannya for

each solution. Its value should be the same as those previously defined at the time of calibration equipment. If not, re-calibrated equipment for the element. Finally, look for solution is not known until the reading is within the transmission or scale meter in accordance with the standard solution, or the 0.01 percent by weight for instruments equipped with a digital readout, and readings for standards in the same way according to the price of calibration. Record average price of the two final readings obtained for a solution that does not known. NOTE 25 The sequence in determining Na2O or K2O is optimal. Though such determination shall be done after the equipment set up and ready to be used for purpose. If the reading exceeds the maximum scale, do one of the move 50 mL solution that has been diluted as prepared in clause 7.1.3.13.1.6). (1) to in a 100 mL beaker or if you want to prepare a new solution using 0.500 grams of cement and 2.5 ml of HCl in the initial addition of acid. In case if the silica was separated from 0.5 g sample of cement, cement treated which has been dehydrated with 1.25 mL of HCl and approximately 20 mL of water, then digest, filter, and wash. For both of the above, add 5.0 mL of mother liquor of calcium chloride before it is diluted with water to mark boundaries. If necessary dilution Further, as specified in paragraph 7.1.3.13.1.4). (3) in this test method. Set appropriate levels of alkaline solution is in point 7.1.3.13.1.6). (2). and multiply by factor of 2 to calculate the percentage of alkali oxides. (3) Procedures for K2O For the determination of K2O repeat the procedure as described in item 7.1.3.13.1.6). (2). For instruments that can read both Na2O and Simultaneously K2O, K2O determination made at the same time with determination of Na2O. 7) Calculation and report Of recording average Na2O and K2O in the unknown sample, report each oxide with 0.01% accuracy.

7.1.3.13.2 Water-soluble alkali NOTE 26 Determination of water-soluble alkali should not be considered as a substitute determination of total alkali in accordance with clause 7.1.3.13.1.2) through 7.1.3.13.1.7). What's more, the method does not assume that all that is in the cement alkali soluble. This procedure is very important to follow carefully because of the limits to the levels of alkaline soluble in water or if to compare a number of cement with a cement based on the levels of water-soluble alkali. 1) Procedure (1) Weigh 25.0 grams of sample put in 500-ml erlenmeyer flask and add 250 mL of water.

Close flask with a rubber cap and shake perfect for 10 minutes at room temperature. Filter through a Buchner funnel fitted with a holder to dry filter paper, filter into a 500-ml flask, using weak vacuum. Do not wash. (2) Remove 50 mL of the diluted solution (NOTE 27) filtrate to in a 100 mL measuring flask and acidify with 0.5 mL HCl (specific gravity 1.19). Add 9.0 mL of mother liquor CaCl2 (63 000 ppm CaO), as described in paragraph 7.1.3.13.1.4). (1), the 100 mL flask, dilute the solution to 100 mL. If this test method requires a more dilute solution, the standard in or both, do the same dilution as in point 7.1.3.13.1.4). (3) (3) Set Na2O and K2O content of this solution as described in item 7.1.3.13.1.6). (2) and 7.1.3.13.1.6). (3). Record ppm respectively in alkaline solution contained in the flask 100 mL. NOTE 27 The solution was diluted from the filtrate taken for analysis should be based on the estimated levels of water-soluble alkali. If the estimated levels of K2O or Na2O more than 0.08% by weight of cement, or if the alkalisoluble unknown water, 50 mL of the diluted solution is given in clause 7.1.3.13.2.1). B) add 1 ml of HCl and evaporation on a hot plate in a beaker 250 mL to about 70 mL. Add 8 mL of mother liquor CaCl2 and transfer sample into 100 mL measuring flask, Rinse the beaker with distilled water. Cool the solution to room temperature and dilute to 100 mL. 2Calculation Calculate the percentage of total alkali-soluble in water, expressed as Na2O, to the nearest 0.01. Total alkali-soluble in water, expressed as follows:

A = B (V x 10) C = D/(V x 10) E = C x 0,658 with: A solution is sodium oxide levels in water (Na2O),%; V is the volume of the original filtrate in a flask 100 mL; B is the concentration of Na2O in the solution contained in a 100 mL flask, ppm; C is potassium oxide soluble in water (K2O),%;

D is the concentration of K2O in the solution contained in a 100 mL flask, ppm; E is equal to the Na2O content in the flask. 7.1.3.14 Manganese oxide 1) Summary of test method In this test procedure manganese oxides with defined volumetric titration sodium arsenite after oxidized manganese in cement sodium metabismutat (NaBiO3). 2) Reagent (1) standard solution of sodium arsenite (1 mL = 0.0003 grams Mn2O3) Dissolve in 100 mL of water 3.0 grams of sodium carbonate (Na2CO3) and then add 0.90 grams of arsenic trioxide (As2O3) heat the mixture late as perfect as possible. If the solution is not clear or contain residues, strain the solution. Cool to room temperature, transfer to a flask measuring and dilute to a volume of 1 liter. Dissolve 0.58 grams of potassium permanganate (KMnO4) into 1 liter of water and Standardise the 0.03 grams of sodium oxalate (Na2C2O4) oksidimetri standards that issued by the National Bureau of Standards (Standards Sample No.. 40 or successor) in accordance with the provisions of the label sodium oxalate. Place 30.0 mL of KMnO4 in 250 mL erlenmeyer flask, then add 60 mL HNO3 (1 + 4) and 10 mL of sodium nitrite (NaNO2, 50 g / L). Boil the solution to evaporate all HNO2. Cool the solution, add NaBiO3 and finally titration with standard solution of sodium arsenite (NaAsO2) as described in clause 7.1.3.14.3). (2). Calculate manganese oxide (Mn2O3) which is equivalent to the solution NaAsO2, in g / mL, as follows:

with: E is equal to the solution NaAsO2 Mn2O3, g / mL; A gram Na2C2O4 is used; B is milliliters of KMnO4 solution required by Na2C2O4; C is NaAsO2 milliliter of solution required by 30.0 mL of KMnO4; 7.08 is the ratio of the molecule Mn2O3 5Na2C2O4 (0.236) multiplied with 30.0 mL of KMnO4.

(2) Sodium metabismutat (NaBiO3) (3) A solution of sodium nitrite (NaNO2 50 g / L) 3Procedure (1) Weigh (1.0 to 3.0) gram sample (NOTE 28) insert into beaker And add 250 mL (5-10) mL of water, then with (6075) mL HNO 3 (1 +4). Boil the mixture to form a perfect solution. Add 10 mL solution of NaNO2 (50 g / L) to the solution above and simmer until evaporated all of nitrous acid (NOTE 29), be careful not volume of the solution to be a little left, causing the precipitation SiO2 in the form of gelatin. If there is a separate part of the SiO2 may can be ignored, but if there is a red or brown residue, use more NaNO2 solution (50 g / L) to enhance decomposition, and then boil it again to remove the nitrous acid. Filter the solution through a porous medium filter paper into a 250 mL erlenmeyer flask and wash filter paper with water. NOTE 28 Number of cement used for the analysis depends on the content of Manganese, ranging from 1 g to 1% to 3 grams Mn2O3 to Mn2O3 0.25% or less. NOTE 29 When NaNO2 added HNO2 evaporation by boiling should be perfectly. If there is manganese in cement, a small amount of NaBiO3 will provide purple. 2The solution must have a volume (100-125) mL. Cool to room temperature. To a solution NaBiO3 add little by little until the number of wholly 0.5 grams, while occasionally shaken. After the addition is complete, the solution shake occasionally for 5 minutes and then add 50 mL HNO 3 (1 33) that has been boiled cold previously to eliminate nitrous acid. Filter the solution through a plate that has been coated Gooch asbestos or carbon or glass filter with the aid of suction. Wash 4 times with HNO3 residue (1 + 33) cool. Immediately titrate the filtrate with standard solution NaAsO2. The end point is reached when the yellow form that is free from brown or purple and does not change with the addition of a solution NaAsO2 excess. 4) blank Create a blank determination, following the procedure and the same amount of reagent, correction of the results obtained in the analysis.

5) Calculation Calculate the percentage of Mn2O3 with 0.01 accuracy as follows:

with: E is equal to the solution of Mn2O3 NaAsO2 g / mL; V is milimiter NaAsO2 required sample solution; S is gram sample used. 7.1.3.15 Chloride 1) Summary of test method In this test method the total chloride content in the manner specified portland cement potentiometric titration with silver nitrate. This procedure can also be used to hardened concrete, slag, and portland cement raw mix. In testing conditions, there is no disturbing elements. NOTE 30 The salts form insoluble silver or silver complex stable in acid solution will interfere with potentiometric measurements, the iodide and bromide can not interfere while fluoride, sulfide salts at usual concentration contained in the material will not interfere because it would decomposed with acid treatment. 2equipment (1) Ion Selective Electrode / chloride ion selective electrode of silver / sulfide, or rodelectrodes coated with silver chloride (NOTE 31), using appropriate comparison electrode. (2) Potentiometer with millivolt scale that can be read up to 1 mV or more accurately potentiometer equipped with reading digital, but not required. (3) A class Buret, 10 mL capacity with 0.05 ml of the scale division. burette type potentiometric, equipped with a regulator drops, better, but not are required. NOTE 31 The electrodes that fit can be obtained from orion Beckman instrument, Leeds and Northup. After studying carefully the instructions of the manufacturer complete solution electrode filler. Silver rod electrodes must be coated with a thin layer of AgCl electrolytic. To coat the electrodes, dip the stems clean silver electrode in a solution of saturated potassium chloride ( 40 g / L) in water and stream of electrical current through electrodes dry cell voltage 1.5 V-6 V. Carbon rod electrode of dry cell

or other appropriate connected to the negative pole tip and dip it in the solution so that the electrical circuit perfectly. If the layer of silver chloride electrode wear, renew return electrode by repeating the above procedure. All the old silver chloride electrodes must be separated from the silver by rubbing the rod slowly using fine sandpaper followed by rinsing the electrode rod with water. 3reagents (1) Sodium chloride (NaCl), primary standard grade. (2) Silver nitrate (AgNO3), reagent grade. (3) Potassium chloride (KCl), reagent grade (which is required specifically for stem silver electrodes). (4) Preparation of the solution (1) standard solution of sodium chloride (NaCl 0.05 N) Dry sodium chloride (NaCl) at a temperature of 105 oC-110oC to severe fixed. Weigh 2.9222 g NaCl dried. Dissolve in water and dilute to exactly 1 liter measuring flask and perfect shake. This solution is the default and need not be standardized more further. (2) standard solution of silver nitrate (AgNO3 0.05 N) Dissolve 8.4938 grams of silver nitrate (AgNO3) in water. Dilute to 1 liter in a measuring flask and shake it perfectly. Standardise against standard solution of 5.00 mL of 0.05 N sodium chloride that has been diluted to 150 mL with water followed by titration test method given in clause 7.1.3.15.4). (4) begins with the phrase "Place the beaker on the magnetic stirrer and so on". Normality is right to be calculated from the average of three determination as the following:

with: N is the normality of AgNO3 laturan; 0.25 is the military equivalent of NaCl (5.0 mL x 0.05 N); V is the volume of AgNO3 solution, mL. Standard solution on the market may be used provided normality checked in accordance with the procedure standardization.

(3) The indicator methyl orange Prepare a solution containing 2 grams of methyl orange in 1 liter of 95% ethyl alcohol. 4procedure (1) Weigh 5.0 g of cement concrete or 10.0 gram sample into a beaker 250 mL (NOTE 32). Dispersed sample with 75 mL of water. Without suspended slowly add 25 mL HNO3 (1 + 1), crushed clots with stirring bar. If the smell of hydrogen sulfide rock is too strong, add 3 ml of hydrogen peroxide 30% (NOTE 33). Add 3 drops of methyl orange indicator and stir. Close beaker with a watch glass and let stand for (1-2) minutes. If yellow to orange color appears at the top of the sediment, solution is not acid enough. Add dilute HNO3 (1 +1) dropwise while stirring so that the color pink or red color is not lost, then add 10 drops excess. Heat the beaker covered quickly to a boil. do not let it boil more than a few seconds. Remove from the hot plate (NOTE 34). NOTE 32 Use 5 grams for example cement, and 10 grams for concrete examples and other materials that have a chloride content of less than 0.15% Cl. For materials that higher chloride levels, reduced the number of instances proportional. These materials do not need to be milled powder. Examples must be ground to escape rough 20 mesh sieve. If the sample is too subtle Silica gel will cause excessive formation during the acid digest nitrates, so the filtering becomes longer. NOTE 33 Slag cement and slag containing high sulphide sulfur can interfere with the determination. NOTE 34 It is important to keep that closed during the beaker pendigestan heating and to prevent loss of chloride evaporation. The use of excessive acid must be avoided as it will accelerate release coating of silver chloride electrodes silver rod. Slightly acidic slurry enough. (2) Wash the rough porous filter paper 9 cm diameter four times with 35 mL of water that uses a vacuum and is equipped with a Buchner funnel 250 mL or 500 mL suction flask attached above. Remove wash and rinse pumpkin once again with a