Sni 15-2049-2004 In English 2p632t

SNI 15-2049-2004

Portland Cement 1.Scope This standard covers the scope, normative references, and definitions, types and use, quality requirements, sampling method, test methods, the requirement of ing 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-μm (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 of quality 5.1 Chemical requirements of portland cement shall meet the following requirements: Table 1 The main chemical conditions Unit in（％）

No.

Commentary

Type Portland cement III IV

I

II

SiO2, minimum

-

20,0 b,c)

-

-

-

2.

Al2O3, maksimum

-

6,0

-

-

-

3.

Fe2O3, maksimum

-

6,0 b,c)

-

6,5

-

4.

MgO, maksimum

5.

8.

SO3, maksimum If C3A < 8,0 If C3A > 8,0 Lost incandescent,maksimum Insoluble Part, maksimum C3S, maksimuma)

9.

1.

6,0

6,0

6,0

2,3

2,3

d)

d)

3,0

2,5

3,0

3,0

1,5

1,5

1,5

1,5

-

-

-

35b)

-

C2S, minimuma)

-

-

-

40b)

-

10.

C3A, maksimuma)

-

8,0

15

7b)

5b)

11.

C4AF + 2C3A or a)

-

-

-

-

25c)

7.

C4AF + C2F, maksimum

3,0

6,0

3,5 4,5 3,0

6.

3,0 3,5 5,0

6,0

V

d)

Note : a)

restrictions chemically based calculations for potential compounds certain not to be construed that the oxide

of potential compounds in pure state. C = CaO, S = SiO2, A = Al2O3, F = Fe2O3, example C3A = 3CaO.Al2O3. 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 so（C4AF+ C2F）and 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 additional physics (Table 4), the chemical condition does

not apply. c)

If the expansion is required because the sulfate listed in the table Additional physical requirements (Table 4), the

chemical condition does not apply d)

Can not be used Table 2 Additional chemical requirement a) No

Unit in（％） Type Portland Cement

Commentary I

II

III

IV

V

1.

C3A, maksimum

-

-

8

-

-

2.

C3A, minimum

-

-

5

-

-

3.

(C3S + 2 C3A) , maksimum

-

58 b)

-

-

-

4.

Alkali as (Na2O + 0,658 K2O), maksimum

0,60 C)

0,60 C)

0,60 C)

0,60 C)

0,60 C)

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

5.2 physics portland cement shall meet the following requirements: Table 3 The main physical requirements No . 1.

Commentary

I

II

III

IV

V

160 280 0,8

160 280 0,8

160 280 0,8

160 280 0,8

160 280 0,8

Fineness： air permeability test，m2/kg with tools： Turbidimeter, min Blaine, min

2.

Type Portland Cement

Immortality: The autoclave expansion，maks％

0 3.

0

0

0

0

strong press： Age 1 day，Kg/cm2，minimum

-

-

120

-

-

Age 3 day，Kg/cm2，minimum

125

100

240

-

80

-

70

150

70a) Age 7 day，Kg/cm2，minimum

200

120a)

Age 28 day，kg/cm2, minimum 4.

175

280

-

-

170

210

-Start, minute, minimum - Finish, minute, maksimum

60 600

60 600

60 600

60 600

60 600

Vicat - Start, minute, minimum - Finish, minute, maksimum

45 375

45 375

45 375

45 375

45 375

Bonding time (alternative methods) with the tool： Gillmore

Note： a)

Compressive strength requirement applies if the conditions of heat of hydration requirements as listed in the table additional physics (Table 4) or if the C3S + C3A requirements as listed in the table additional chemicals required (Table 2). Table 4 Additional physical requirementsa) No .

Commentary

1.

Binding of apparent penetration of the end， ％minimum Hydration heat Age 7 day，kal/gram，ma ks

2.

Type Portland Cement I

II

III

IV

V

50

50

50

50

50

-

70b)

-

60

-

Age 28 day，kal/gram，ma ks compressive strength： Age 28 day，Kg/cm2， minimum

-

-

-

70

-

-

280

-

-

-

expansion due to sulfate 14 day，％maksimum 5. Air content of mortar， ％volume，maksimum Note：

-

220b)

-

-

0,040

12

12

12

12

12

3.

4.

a)

Additional physical requirement applies only if specifically requested. When the 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. b)

6 . Way Sampling 6.1 Description of 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 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 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

NO. 1.

Lapse of time (days)

Compressive strength (the age test, day) Chemical analysis, autoclave, normal consistency Vicat apparatus, the apparatus blaine fineness, fast rigid

8

paste method. 2.

Compressive strength (test results 3 days)

3.

Compressive strength and heat of hydration (age 7 days of test results)

10 14

4.

Expansion due to sulfate (age test results 14 days)

21

5.

Compressive strength and heat of hydration (test results

35

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.

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 μm (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

Maximum difference of The average twodetermination by SRM Certificate (unit in%)

1.

SiO2 (Silikon dioksida)

0,16

± 0,2

2.

Al2O3 (Aluminium oksida)

0,20

± 0,2

3.

Fe2O3 (Besi(III) oksida)

0,10

± 0,10

4.

CaO (Kalsium oksida)

0,20

± 0,30

5.

MgO (Magnesium oksida)

0,16

± 0,2

6.

SO3 (Sulfur trioksida)

0,10

± 0,1

7.

HP（缺少白炽灯）

0,10

± 0,10

8.

Na2O (Natrium oksida)

0,03

± 0,05

9.

K2O (Kalium oksida)

0,03

± 0,05

10.

TiO2 (Titanium dioksida)

0,02

± 0,03

11.

P2O5 (Posfor pentaoksida)

0,03

± 0,03

12.

ZnO (Seng oksida)

0,03

± 0,03

13.

Mn2O3 (Mangan oksida)

0,03

± 0,03

14.

S (Sulfida)

0,01

-

15.

Cl (Klorida)

0,02

-

16.

IR（Insoluble part）

0,10

-

17.

FL（Calcium oxide-free）

0,20

-

18.

Sol ALK (Alkali-soluble

0,75/w

-

19.

in water CHL sol (organic compounds

0,004

-

soluble in chloroform) 7.1.1.2 Alternative test methods 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 1）Equipment （1）Equipment 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. （2）Laboratory 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. 2）Materials 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. （1）The 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 acid（CH3COOH）99.95％ hydrochloric acid（HCl）1.19 b.j hydrofluoric acid（HF）48％ nitric acid（HNO3）1.42 b.j phosphoric acid（H3PO4）85％ sulfuric acid（H2SO4）1.84 b.j Amonium hidroksida（NH 4 OH）0.90 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. (2）Indicator 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. 1）major 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

2）minor 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) 3）Separate 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 1）Summary 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. 2）Reagents Solution of ammonium nitrate (NH4NO3 20 g / L). Solution of sodium hydroxide (NaOH 10 g / L). 3）procedure (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. 4）calculation Calculate levels of insoluble parts with accuracy to 0.01% % insoluble part = heavy sediment

X 100

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). 1）Silicon 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. 2）Reagents Ammonium chloride (NH4Cl).

Hydrochloric acid (HCl). Hydrochloric acid (HCl) (1 +99). Nitric acid (HNO3). Sulfuric acid (H2SO4) (1 +1). Hydrofluoric acid (HF). （3）procedure 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 2）Transfer 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 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.

3）If 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)

4）If 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. 5）In 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. 6）Perform a blank determination using the reagents and test methods the same result as a correction into in the calculation. （4）Calculation 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. 2）Silicon 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. (2）Reagents Sodium carbonate (Na2CO3). Hydrochloric acid (HCl). Hydrochloric acid (HCl) (1 +3). Hydrochloric acid (HCl) (1 +99). Hydrochloric acid (HCl) (1 +1).

（3）procedure 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. 2）Evaporation 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. 3）Evaporation 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) 1）Summary 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. 2）reagents Hydrochloric acid (HCl SG 1.19). Hydrochloric acid (HCl) (1 +2). Ammonium hydroxide (NH4OH) (1 +1). Ammonium nitrate (NH4NO3). 3）procedure (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. （2）Collect 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).

（3）Place 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. （4）Perform a blank determination using reagents and a same result as a correction into in the calculation. 4）Calculation Calculate R2O3 levels with accuracy of 0.1% %R2O3 =

heavy sediment heavy sample

X 100

7.1.3.4 Iron (III) oxide (Fe2O3) 1）Summary 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. 2）reagents (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.

3）procedure 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. 4）blank 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. 5）Calculation 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) 1）Summary 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. 2）Equipment 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). 3）Reagents (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. （3）Standard 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. （5）Phosphate 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. 2）reagents (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. （4）Filter 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. （5）Place 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 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. 4）blank 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. 5）calculation 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. 3）Procedure 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). 4）Blank 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 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. （3）blank 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 cium chloride amoniakal Dissolve 15 g of cium 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. （4）procedure 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). （5）calculation 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 1）Portland 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. （3）Calculation 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. 2）Cement 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

（3）calculation 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 1）alkali 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. 3）Reagents 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. 4）preparation 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. （3）standard 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. 5）calibration In accordance with the manufacturer's operating instructions 6）procedure (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. （2）Procedures 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. 2）Calculation 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) 3）Procedure (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. （2）The 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. 2）equipment (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. 3）reagents (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. 4）procedure (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 little water. Replace the vacuum equipment and filtered sample solution. Rinse the beaker and filter paper twice with use less water. Transfer the filtrate from the flask into the beaker original can be used (NOTE 35). Cool the filtrate to room temperature. The volume should not exceed 175 mL. (3) For instruments equipped with a digital readout needs to establish the approximate "equivalence point" by dipping electrode into a beaker filled with water and adjust the instrument so readings less than 20 mV over rencah middle of the scale. Record the millivolt meter readings. Move the beaker and wipe the electrode with blotting paper. (4) In the example that has been desired (NOTE 36) beaker of grain 7.1.3.15.4). (2) carefully pipette 2.00 mL standard

solution of NaCl 0.05 N. Place the beaker on the magnetic stirrer and insert into it TFE-coated magnetic stirring bar fluorocarbon. Dip the electrode into the solution, be careful about not mixing electrodes, start early with low speed stirring. Place the burette 10 ml dropper, which has been filled up to mark boundaries with a standard solution of silver nitrate above 0.05 N beaker (NOTE 37). NOTE 36 It is advisable to maintain a constant temperature during the measurement takes place because the solubility of silver chloride vary quite greatly to the temperature at low concentrations. NOTE 37 If - burette place dispense the solution, there is a trickle stick must be rinsed in a beaker with a few milliliters of water every time after the addition peniter. (5) Titration little by little, record the amount of nitrate standard solution of 0.05 N required to obtain readings to milivoltmeter 60.0 mV of the equivalence point specified in the water. (6) Continue the titration, whenever penambahakan volume of 0.20 mL painter. Record buret readings and readings milivoltmeter in columns 1 and 2 in recording record form that consists of 4 columns as shown in Appendix A. Each time adding painter let the electrodes reached, equilibrium with the sample solution. Experience has shown that proper readings are obtained when minimum scale reading does not change within 5 seconds (usually in time 2 minutes) The closer to the equivalent point, the addition of AgNO3 solution in an amount the same will lead to larger changes in the reading milivoltmeter. Past the point of equivalent changes will decrease again. Continue adding titration up to three more after the equivalent point estimated to have recorded. (7) Calculate the difference in readings in millivolts from the addition of another painter and enter the value in column 3 of the record form. (8) Calculate the difference in column 3 of the addition of one to the next and enter the result in column 4. Equivalent point of the titration will be in the interval of a maximum of 4 MV recorded in column 3. Equivalent point can be interpolated from the data listed in column 4 as shown in Appendix A. 5）blank Create a blank determination using 75 ml of water instead of sample, follow the same procedure as in paragraph 7.1.3.15.4). (1). begins with the sentence "Without suspended slowly add dst". Correction of analytical results obtained by subtraction of blank (NOTE 38). NOTE 38 For the analysis of non referees, blank determination should not be done.

6）calculation Calculate the percentage of chloride with 0.001% accuracy as follows:

with: V1 is a milliliter of 0.05 N AgNO3 solution used for titration of sample (point equivalent); V2 is a milliliter of 0.05 N AgNO3 solution used for blank titration; N is the exact normality of the 0.05 N AgNO3 solution; W is the weight of sample, grams. 7.1.3.16 Organic compounds that are soluble in chloroform 1) Summary of test method. The test method is designed specifically for the determination of resin and tallow in vinsol portland cement, although there are mineral oil, resin, calcium stearate, and other fatty acid compounds and some organic compounds are included in the this designation. Be careful at work throughout this procedure. This test method can be used to cements other than portland cement. Although cement contains parts that are not high enough soluble, emulsion would separate slowly, and agitation should not be too strong so more use of chloroform and washing more often.

2) Reagent (1) Chloroform If the blank determination as described in item 7.1.3.16.4) exceeded 0.0015 grams of chloroform should be distilled before use. Chloroform recovered may be a bit sour but can be reused shaking with an acid solution of the sample in 1 liter separating funnel. Chloroform was used to wash the filter and separator should be a fresh or has been distilled. (2) Tin (II) chloride (SnCl2). 3) Procedure (1) Place 40 grams of cement in the separator funnel Squibb 1 liter (NOTE 39) and stir it with 250 ml of water were

added in 2 equal parts much. Beat vigorously with a soon to produce a perfect decomposition. Then add the second and shake again. Simultaneously quickly add 185 mL into which was dissolved 10 grams of SnCl2 (NOTE 40) immediately close the funnel, the funnel upside down and shake in a circular motion for a few seconds to loosen and dispersing cement, carefully avoiding the huge pressure because too strong agitation is not required. Remove the pressure immediately by opening and closing valves cover. Repeat shaking and spending pressures to cement decomposes perfectly. If necessary, break the clumps of cement are still there with the trunk glass stirrer. Immediately cool to room temperature by placing the mouthpiece under water flow faucet. NOTE 39 The use of fat to lubricate the valve cover and glass cover the funnel separator should be avoided. Moisten glass cover with water before use that will facilitate the work NOTE 40 The purpose of the addition of SnCl2 is to avoid oxidation of sulfide sulfur to elemental sulfur, which is soluble in chloroform. (2) Add 75 ml of chloroform into the solution, separating funnel lid, shake vigorously for 5 minutes, and let stand for 15 minutes to separate the water and chloroform. Chloroform layer located at the bottom bagiah removed and disposed of Squibb in 125 mL separator funnel, including foam (NOTE 41) and a few milliliters of water layers, make sure all the layers of foam has been removed. Keep the number of water-borne coating as little as possible, because the excess water too much in 125 mL separating funnel can cause extraction imperfect of foam and emulsion may cause subtle. Beat the other 250 mL separating funnel containing 50 mL of water and a few drops HCl. Shake the separator funnel the same as in a state of 250 mL separating funnel first. If the chloroform separates, stream into the flat bottom boiling flask (NOTE 42), be careful not to get water into the boiling flask. NOTE 41 Usually shaped like a foam face. May contain compounds organic soluble in chloroform after shaking the funnel separator, where comparison of the water with chloroform. Maybe the foam can be concentrated and be in a little volume by rotating separator funnel slowly after the foam is applied to the narrow part of the funnel separator. NOTE 42 Then the liquid is distilled, the cover of cork or rubber should not be heated, soil analysis 250 mL flask or 300 mL, equipped with tube condenser can be used. Condenser tube has a curve near the neck and the jacket cooling water (Water Cooling Jacket). Chloroform can be recovered used again as in point 7.1.3.16.2). (1).

（3）Add 25 ml of chloroform to the solution is in the separator funnel 1 liter original, and do according to clause 7.1.3.16.3). (2) save dishwater initially in a 250-ml separating funnel. Repeat using 25 mL of chloroform. Distillation combined chloroform extracts pumpkin in boiling until the volume is reduced to a (10-15) mL. Filter the solution separated into 100 mL beaker or cup amplifier platinum (NOTE 43) of known weight through a porous medium filter paper and then rinse with fresh chloroform. Rinse the flask and wash the filter paper with a bit of fresh chloroform several times. Evaporation extract at low temperature not more than 63oC until dry. (NOTE 44) and reheat in the oven at a temperature (57-63) ° C for 3 min. Dry air stream into the container for 15 seconds, cool and weigh. Repeat heating and weighing up to 2 times in a row weighing the difference is not more than 0.0010 gram. Weighing the results of the last two higher weight is taken as the truth. NOTE 43 cup vaporizer used because platinum is better achieved faster equilibrium temperature. Beaker when used, should be allowed to reach temperature equilibrium at least 20 minutes before weighed. NOTE 44 Be careful when filtering the extract as many organic compounds soluble in chloroform evaporates when heated too long though heated at moderate temperatures. When given protection from dust accumulation, the solution can be evaporated at room temperature when left overnight. If desired rapid evaporation, the solution can be evaporated on hot plate at low temperature with a given stream of dry air through a glass tube internal diameter of 10 mm and a thickness of approximately 3 mm. Then lift the glass of Plate heat and dry air jetting proceed slowly until visible residue dried and then continue with the dry air flow faster over the past 5 minutes at room temperature before the beaker is placed in an oven at a temperature of (57-63) o

C.

Each 3-minute warm-up period in the oven, hot air stream into the container for ± 15 seconds before it is weighed. Dry air can be ed after drying agents such as calcium chloride or sulfuric acid, followed by drying agents have a high efficiency, such as magnesium perchlorate or calcium sulfate anhydrous, carefully avoid dust entrainment of air by air. Besides using compressed air, which is often contaminated with oil, dirt and moisture can also be done by putting a chloroform solution under the hood glass and air flow through drying agents using tools aspirator or pump vacuum. If there are known only vinsol resin, residue more stable and can be heated temperature (100-150) oC, but not at (5763)oC ie when there are also elements other unstable organic to remove all remnants of chloroform may be left behind. 4）blank Make a blank determination. Pijarkan 40 grams of semen samples at temperatures (950-1000)° C for 1 hour (NOTE

45) and puree again. Treat example has dipijarkan using procedures and a number of The same reagent in the analysis, the results obtained correction. NOTE 45 Be careful working so organic compounds burn completely. Sprinkle examples in platinum 100 mL evaporating dish and encouraged to wear muflle furnace not available, the type burners Maker with high temperatures can be used. Stirring a perfect example should be done periodically every 5 minutes if using a burner. 5）calculation Calculate the percentage of organic compounds that are soluble in chloroform to 0.001 accuracy by multiplying the sample weight in grams of the residue (NOTE 46) to 2.5 (100 divided by the weight of the example used 40 grams). NOTE 46 If the organic compounds contained in the semen is tallow residue is fatty acids derived from tallow hydroxide is in the hot acid solution and the weight must be multiplied by 1.05 to obtain the weight actual tallow glycerides in it. If a compound is calcium stearate prganik origin, then the residue is stearic acid, and its weight is multiplied by 1.07 to obtain the actual weight of the calcium The stearate. 7.1.4 Alternative test methods (Optional) 7.1.4.1calcium oxide 1）Summary of test method The test method covers the gravimetric determination of CaO, SiO2 and groups are ammonium hydroxide separated, followed by precipitation of calcium as oxalate. The precipitate is converted into CaO with pemijaran and weighed. Strontium, usually found in portland cement as a minor element, settles with calcium as the oxalate and subsequently calculated as CaO. If SrO content is known and the correction of CaO to SrO desirable for example, for research purposes or to compare the results with the SRM certificate values, CaO obtained by this test method can be corrected by subtraction percentage of SrO. In determining a correction to meet the specifications of cement SrO for CaO not needs to be done. 2）Procedure (NOTE 47) Acidify the combined filtrate from the determination of ammonium hydroxide groups on the grain 7.1.3.3.1) to 7.1.3.3.4) if necessary, kisatkan to a volume of approximately 200 mL. Add 5 ml of HCl, a few drops of methyl red indicator solution and 30 mL of solution

Ammonium oxalate warm (50 g / L) (NOTE 7). Heat the solution at a temperature (70 - 80)oC and add NH4OH (1 +1) dropwise while stirring until the color changes from red to yellow (NOTE 8). Let the solution without further heating for 1 hour (not more), with stirring occasionally for 30 minutes. Filter by using paper fine filter and wash with a solution of ammonium oxalate sufficiently cold (1 g / L). Save the filtrate and washing water. NOTE 47 If the analysis is performed to meet the specifications of the possibility of manganese present in sufficient quantity will cause the percentage of magnesium determination alternative test method exceeds the specification requirements, Mangan should be separated as described in paragraph 7.1.3.9.3.) (2) prior to determination of CaO with alternative methods. Transfer the precipitate and filter paper into a beaker before. Dissolve the precipitate oxalate in 50 mL of hot HCl (1+4) and destroy the filter paper. Dilute to 200 mL with water, add a few drops of methyl red indicator and the calcium oxalate precipitate by acid solution with equipment NH4OH solution as described in paragraph 7.1.4.9.3.) (1).Allow the solution to 1-2 hours, strain and wash as before. Combine the filtrate obtained and stored for appropriate determination of MgO grain 7.1.3.10.3), dried sediment in a known weight krusibel lid. Carbonation paper without a flame, burning carbon at a temperature as low as possible, eventually krusibel pijarkan with lids tightly in an electric furnace at a temperature of (1100-1200)oC. Cool in a desiccator and weigh as CaO. Ignition Repeat until the weight remains. 3) blank Create a blank determination, using procedures and a number of reagents together in the analysis and correction of the results obtained. 4) Calculation Calculate the percentage of CaO to the nearest 0.1 by multiplying weight in grams of CaO with 200 (100 divided by the weight of the examples used 0.5). Correction to% CaO to SrO, if desired, with a reduction in percent SrO. 7.1.4.2 Magnesium oxide volumetric method 1) Summary of test method This test method is suitable volumetric procedure for use when setting silicon dioxide (SiO2), aluminum oxide (Al2O3), iron (III) oxide (Fe2O3), and calcium oxide (CaO) is ignored. 2) Reagent (1) A solution of ammonium nitrate (20 g NH4NO3 / L)

(2) A solution of ammonium oxalate (50 g / L) (3) Solution Hidroksiquinolin Dissolve 25 grams of 8-hidroksiquinolin in 60 mL of acetic acid. When the solution has completely dissolved, dilute to 2 liters of cold water. Temperature milliliters of this solution is equivalent to 0.0016 grams of MgO. (4) standard solution of potassium bromate-potassium bromide (0.2 N) Dissolve 20 grams of potassium bromide (KBr) and 5.57 grams of potassium bromate (KBrO3) in 200 mL of water and dilute to 1 liter. Set the ratio of the concentration of this solution to a solution of 0.1 N Na2S2O3 in point 7.1.4.2.2). (5) as follows: At 200 mL of water in 500-ml erlenmeyer flask add 25.0 mL of solution KBrO3-KBr 0.2 N. Add 20 ml of HCl, shake, and immediately add 10 mL Potassium Iodide (KI) (250 g / L). Shake and titrate immediately with Na2S2O3 solution until the solution almost colored. Add 2 ml of starch solution and titrate until the blue color disappeared. Calculate the ratio of the concentration of the solution against KBrO3-KBr solution of Na2S2O3 by dividing the volume of Na2S2O3 solution with a volume KBrO3-KBr used in the titration. （5）Potassium iodide standard solution (0.1 N) Dissolve 25 grams of sodium thiosulfate (Na2S2O3.5H2O) in 200 mL of water, add 0.1 grams of sodium carbonate (Na2CO3), and dilute to 1 liter. Leave for at least 1 week. Standardise this solution immediately against primary standard potassium bichromate (K2Cr2O7). One milliliter of solution 0.10 N Na2S2O3 equivalent to 0.000504 grams of MgO. （6）starch solution In 500 mL of boiling water add cold suspension of 5 grams of starch that can be dissolved in 25 mL of water, cool the solution to room temperature, add all made cold solution of 5 grams of sodium hydroxide (NaOH) in 50 mL of water, add 15 grams of KI, and the perfect mix. 3）procedure (1) Dispersikan 0.5 grams (NOTE 48) semen sample in a 400 mL beaker with 10 mL of water, while shaken, as well as add 10 ml of HCl. Immediately dilute to 100 mL. Heat slowly and destroy any coarse particles with rod tipped to unravel perfectly flat, add 2 or 3 drops of HNO3 and heat to boiling (NOTE 49) NOTE 48 If ammonium hydroxide group SiO2 and CaO separated and determined in accordance with the appropriate

method for the reference and test methods Alternatively, the filtrate is left can be used for determination of MgO as described in point 7.1.4.2.3) (1) after the words "Add 5 ml of HCl dst" of grain 7.1.4.2.3) (2) NOTE 49 In the case of cement containing blast-furnace Slag or some significant sulphide sulfur, add 12 drops of HNO3 and simmer for 20 minutes to oxidize the iron and eliminate sulfide. （2）Add 3 drops of methyl red indicator to the solution and then added NH4OH until the solution is yellow. Heat the solution to boiling and continue boiling for (50-60) seconds. If difficulties arise due to bumping the boiling solution Ammonia, in the period pendigestan for 10 minutes on the steam bath, or above the heating plate having the same temperature can be used as substitute for further boiling for 50 seconds -60 seconds on combustion. Remove from burner, steam bath, or heating plate and let to precipitate down. Use porous medium filter paper, immediately strain the solution, wash the precipitate two NH4NO3 times with hot (20 g / L), and save the filtrate. Move precipitate with filter paper into a beaker and dissolve with 10 ml of HCl (1 +1). Destroy the filter paper. Dilute up to ± 100 mL and heat until boiling. The precipitate is filtered again and wash hydroxide as above. Combine the filtrate and washing water deposition first, keep the volume is not exceed 300 mL (NOTE 50). Add 5 ml of HCl, a few drops of solution methyl red indicator and 30 ml of hot ammonium oxalate (50 g / L). Heat the solution at (70-80) oC and add NH4OH dropwise (1 +1), while stirring, until the color changes from red to yellow (NOTE 51). Let the solution without further heating for 15 minutes over bath steam. NOTE 50 In this case the cements containing blast furnace, or considered contains significant Mangan, acidify with HCl, estimated to be 100 mL, and separate manganese, as described in clause 7.1.3.9.3). (1) Add 10 mL - 25 mL reagent 8-hidroksiquinolin (NOTE 51) and 4 mL NH4OH/100 mL solution. Stir the solution on a mechanical stirrer machine for 15 minutes, remove from heat and allow to precipitate down (NOTE 52). Filter solution using porous medium filter paper and wash the precipitate with NH4OH (1 +40). Dissolve the precipitate with (50-75) mL hot HCl (1 +9) in a 500 mL erlenmeyer flask. Dilute the solution results obtained up to 200 mL and add 15 ml of HCl. Cool the solution to 25° C and added with a pipette or burette (10-35) mL KBrO3 - 0.2 N KBr (NOTE 53). Stir the solution and let stand for about 30 seconds to convince brominated perfect. Add 10 ml of KI (250 g / L). Stir the solution obtained with good and titrate with 0.1 N Na2S2O3 solution until the

yellow color of iodine pale. At this stage, add 2 ml of starch solution and titrate the solution until blue color disappeared. NOTE 51 Excess reagent 8-hidroksiquinolin necessary to avoid low MgO results, but if too much will give results higher. The instructions below should be used to determine the amount of reagent is added. Table 7 Comparison of the amount of reagent grade MgO required Estimated levels of MgO，

Estimated amount of reagent

％ 0 – 1,5

required, mL 10

1,5 – 3,0

15

3,0 – 4,5

20

4,5 – 6,0

25

NOTE 52 In an interval of 1 hour deposition should be screened. If longer led to high yields. NOTE 53 Number KBrO3-KBr standard solution should use the following list

Table 8 Comparison of MgO content with the amount of the standard solution Estimated levels of MgO，

Estimated amount of reagent

％ 0–1

required, mL 10

1–2

15

2–3

20

3–4

25

4–5

30

5–6

35

4) blank Create a blank determination, using procedures and a number of reagents same, and the correction results obtained in the analysis. 5) Calculation Calculate the percentage of MgO to the nearest 0.1 as follows: (NOTE 54) % MgO = E (V1R – V2) x 200 with: E is equal to the solution of Na2S2O3 MgO, g / mL; V1 is a milliliter of solution KBrO3 - KBr used; R is the ratio of the power of KBrO3 solution - the solution of Na2S2O3 KBr; V2 is the solution of Na2S2O3. used, mL; 200 is 100 divided by weight of sample used (0.5 grams). NOTE 54 VI R shows the volume of Na2S2O3 solution. which is equivalent to the volume KBrO3-KBr solution used, V2 indicate the amount required by Na2S2O3.yang KBrO3-KBr advantages that are not reduced by magnesium oksiquinolat. 7.1.4.3 Titanium dioxide 1) Summary of test method Test methods dioxide (TiO2) is determined by comparing the colorimetric color intensity titanium peroxide solution in the sample to the intensity of color titanik book sulfuric peroxide solution. 2) Disturbance Elements of a bully in the peroxide method for TiO2 is vanadium, molybdenum, and chromium. In small amounts can cause disruption to other elements in the cement therefore fusion with Na2CO3 7.1.4.3.5). (4) and extraction with water is required. 3) Equipment colorimeter Equipment shall consist of the type of colorimeter Kennicou or Duboscq, or Another colorimeter or spectrometer designed to measure light transmittance, and can be used for measurement at a wavelength of 400 nm-450 nm. 4) Reagent (1) Ammonium chloride (NH4Cl). (2) Ammonium nitrate (NH4NO3 20 g / L). (3) A solution of iron (II) sulfate (1 mL = 0.005 g Fe2O3).

Dissolve 17.4 grams of iron (II) sulfate (FeSO4.7H2O) in water containing 50 mL H2SO4 and dilute to 1L. One milliliter is equivalent to 1% Fe2O3 in 0.5 gram sample. (4) Hydrogen peroxide (30%). Concentrated hydrogen peroxide (H2O2). (5) Sodium carbonate (20 g / L Na2CO3). (6) Sodium or potassium pirosulfat (Na2S2O7 or K2S2O7). (7) titanik sulfate standard solution (1 mL = 0.0002 g TiO2). Use of raw TiO2 provided by the National Bureu of Standards (eg, 154 or its successor standard). Dry for 2 hours at (105 -110) oC. Move heavy TiO2 (0.20 to 0.21) g in 125 mL glass philips chemistry. Add 5 grams of ammonium sulphate ((NH4) 2SO4) and 10 mL H2SO4 into beaker and enter a short-stemmed glass separating funnel into the beaker mouth. Heat the mixture to a boil while continuously playing in the pumpkin flame. Continue heating until the solution is completely dissolved and ineffective No part of the material attached to the walls of the pumpkin (NOTE 55). Cool and immediately pour the solution into 200 mL of cold water while stirred vigorously. Rinse the flask and funnel with H2SO4 (1 + 19), stir, then let stand solution and washing water at least for 24 hours. Strain into measuring 1 liter flask, wash filter perfectly using H2SO4 (1 +19), dilute to mark boundary with H2SO4 (1+19), and shake. NOTE 55 Although there is little residual TiO2, it will not interfere when procedure is implemented. Calculate equality TiO2, from titanik sulfate solution, g / mL, as follows:

with: E is the equality of TiO2, from a solution of Ti (SO4) 2, g / mL; A gram is TiO2, which is used raw (correction for loss on drying; B is the percentage of TiO2, raw as stated in the certificate issued by the National Bureau of Standards (NBS), divided by 100; 1000 is milliliters of solution in the measuring flask. 5) Procedure

(1) Mix with a perfect 0.5 grams and 0.5 grams of semen samples NH4Cl in 50 mL beaker, cover the beaker with a watch glass, and add the carefully 5 mL HCl. Allow the acid to flow down past the lip of the beaker with a lid. After the chemical reaction subside, lift the lid, stir the mixture with a rod glass stirrer, cover again (NOTE 56) during pendigestan, stirring once again destroy the contents of the remaining clumps to facilitate cement decomposes perfect. Put a porous medium fast filter paper into the funnel and move sediment into the filter paper. Scrub the wall in chemistry class with a rubber policeman and rinse beaker and policemannya. Wash the filter paper two or three times with hot HCl (1 +99), and then with a little hot water as much as ten or twelve times, let each time wash water to run out. NOTE 56 hot plate can be used as a substitute for the steam bath. If The device is equipped with a thermostat so that the heat generated near hot steam bath. (2) Transfer the filter paper and residue into the krusibel (NOTE 57), drained and ignition slowly until the carbon from the filter paper burn completely without flame. Treat SiO2 obtained with 0.5 mL-1 mL water, 10 mL HF, and 1 drop H2SO4, and uapkan careful to dry. (NOTE 58). NOTE 57 If a shorter procedure desirable for purposes other than the way Test referee, usually with little accuracy ignore such procedures grain 7.1.4.3.5). (2) can be eliminated. NOTE 58 When determining SiO2 desirable addition to the determination TiO2, SiO2 can be treated with HF as the posterior 7.1.3.2. (3) to 7.1.3.2 (4) (3) Heat the filtrate to boiling and add NH4OH until the solution became is really alkaline, shown with the smell of ammonia. Add a little pulp filter paper into a solution and simmer for (50-60) seconds. Let the precipitate formed, filtered through filter paper porous medium, and washing twice with hot NH4NO3 solution (20 g / L). Place the sediment in the SiO2 krusibel its been treated with HF and ignition slowly until depleted carbon from the filter paper. NOTE 59 When determining the desired class of ammonium hydroxide TiO2 additions to the temperature, precipitation and ignition may be made as in 7.1.3.3.3.) (1) through 7.1.3.3.3). (4) However, krusibel must contain residue of treated SiO2 with HF unless the state allows to eliminate it as shown in the NOTE 58 （4) Add 5 grams of Na2CO3, into krusibel and melting during (10-15) minutes (see "Hearing"). Cool, separate the melt from krusibel and transfer to a beaker small.

Krusibel Wash with hot water using a rubber policemen. Digest melt and cleaning up shattered melt then strain through a porous filter paper medium diameter of 9 cm and wash several times with Na2CO3 (20 g / L) Discard the filtrate, place the sediment in krusibel and slowly ignition carbon from the filter paper to burn completely. Add 3 grams Na2S2O7 or K2S2O7 into krusibel and heat to incandescent until the residue dissolved in molten (NOTE 60). Cool and dissolve collection fused into water containing 2.5 mL of H2SO4. If you need to reduce the volume of solution (NOTE 61), filtered into a volumetric flask 100 mL through the filter paper 7 cm diameter porous medium and washing with hot water. Add 5 mL H3PO4 and cool the solution with water, and shake perfectly. NOTE 60 Begin heating with caution because pirosulfat (also known as molten bisulfate) are splashed at the beginning of the heating due to H2SO4. Avoid high temperature or for too long heating is not required because the fused pirosulfat can damage the platinum. Wear pirosulfat are not splashed by providing partial heating pirosulfat in krusibel to remove excess H2SO4. and break times fused cold. NOTE 61 If the solution is evaporated to the volume a bit and left it being cold, can lead sulfate precipitate difficult to redissolve. In the event of excessive evaporation, do not let it be cold, but add hot water and digest on the steam bath or need heating up all precipitate dissolved again, with still a slight possibility that SiO2 can not dissolve back. NOTE 62 From time to time, hydrogen peroxide will decompose. The strength can be determined by adding a certain amount into 200 mL of cold water and 10 mL H2SO4. (1 +1) and then titrated with a standard solution potassium permanganate (KMnO4) were prepared according to clause 7.1.3.9.2). (2). If the standard solution contains 0.0056357 grams KMnO4 / mL, 49.5 mL of the solution is required by 0.50 mL of 30% H2O2. reference standard in 100 mL measuring flask, depending on the type of colorimeter is used. Into each solution, add 3 grams of Na2S2O7 or K2S2O7 the was dissolved in water, then add a solution that Fe2SO4 equivalent Fe2O3 containing 0.5 grams of cement, 2.5 mL H2SO4 and 5 mL H3PO4 (NOTE 63). When the solution is at room temperature, add 1.0 mL of 30% H2O2, dilute to the mark with water and the boundary perfect shake (NOTE 64). NOTE 63 color caused by the solution of Fe2 (SO4)3 most influence bleaching H2SO4, H3PO4 and salts of alkali metal ions and ion peritanic. The sequence must be followed to obtain high accuracy. However when wanted a shorter procedure for purposes other than analysis of referees, pirosulfat addition, FeSO4 and H3PO4 solution to the reference solution can be omitted when Fe2O3 in the semen sample is less than 5%. It can lead to slightly reduced accuracy.

NOTE 64 color develops rapidly and is stable for some time, but if the peroxide solution was left in a long time, bubbles of oxygen will appear and disrupt the color comparison. If the contents of the first tube stirred, possibility of fine bubbles are formed which must be left to clear before the comparison is performed. Comparison between the standard solution and the sample should be done in intervals of no more than 30 minutes after the addition of H2O2. (6) Compare the color, the light transmittance or absorbance of the sample solution with a reference standard solution. How to compare the solution color or transmittance measurement or absorbance depends on the type of equipment (see clause 7.1.4.3.5). (7) through the 7.1.4.3.5). (9) and must conform to a given tools by the manufacturer. When the cement peroxide solution peroxide solution compared to a standard, that from a single standard solution can not cover all areas TiO2 levels required. The difference in volume or depth for both liquid should not be more than 50% of the price of the smallest. All solutions should contain H2SO4, H3PO4, Fe2 (SO4)3 and persulfate were concentration has been established, unless such undesirable circumstances accordance with the NOTES 55. (7) the type colorimeter Kennicott By using a piston (plunger) in a reservoir solution of peroxide Raw, set the amount of the solution to deliver the intensity of light ed same color with peroxide solution examples. (8) type colorimeter Duboscq. Up or down torque of the bowl so the two solutions provide intensity of the same color when viewed from above. Comparison of color can be done visually or photoelectric. (9) colorimeter designed to measure light transmittance. Measurements should be taken at a wavelength of 400 nm-450 nm can be performed either visually or photoelectric. In most colorimeter type, the equipment was calibrated with standard solution and the calibration curve shows the relationship between light transmittance or absorbance of the TiO2 levels (which have been prepared ahead of time). 6) blank Create a blank determination, following the procedure and some of the same reagents and correction of the results obtained in the analysis. 7) Calculation Calculate the percentage of TiO2 to the nearest 0.01. When the colorimeter is designed to measure the transmittance of light used: read TiO2 percentage of the curve calibration showing the relationship of light intensity on levels of TiO2. When compared to peroxide solution example one reference standard solution, calculate the percentage of TiO2 as

follows (NOTE 65) For type colorimeter Kennicott: %TiO2 = (100 VE/S) x (D/C) To colorimeter Duboscq type: %TiO2 = (100 VE/S) x (F/G) with: V is milliliters of standard solution of Ti(SO4) 2 in standard peroxide solution; E is the equality of TiO2 standard solution Ti(SO4) 2, g / mL; S is gram sample used; C is the total volume of peroxide reference standard solution, mL; D is the volume of standard solution that is comparable to the reference peroxide solution peroxide sample, mL; F is the depth of the reference standard peroxide solution by the light; G is the depth peroxide solution samples taken by the light. NOTE 65 The difference between D and C or between F and G can not exceed 50% The smallest price 7.1.4.4 Fosfor pentaoxide 1) Summary of test method In this method, the volumetric phosphorus determined by precipitating phosphorus as ammonium fosfomolibdat and ditirasi with NaOH and H2SO4. 2) Reagent (1) A solution of ammonium molybdate Prepare a solution in accordance with Section 7.1.3.5.3). (1) (2) Ammonium nitrate (NH4NO3) (3) Potassium nitrate (10 g / L) Dissolve 10 grams of potassium nitrate (KNO3) in water that has been free of CO2, Dilute to 1 liter (water released from CO2 by boiling). (4) standard solution, sodium hydroxide (0.3 N) Dissolve 12 grams of sodium hydroxide (NaOH) in 1 liter of cold water that has been free CO2 (CO2 released from the

water by boiling). Add 10 ml of saturated solution of barium hydroxide (Ba (OH)2) are fresh and has been filtered. Shake the solution on a regular basis for a few hours, and strain. Keep contamination of CO2 from the air. Standardise the solution against potassium acid phthalat (No. standard example. 84) or benzoic acid (sample No. standards. 39) that has been provided by the National Berau Standards in accordance with the instructions that complement the standard material them. Calculate equality pentaoksida phosphorus (P2O5) (NOTE 66) of the solution (g / L), as follows: E = N x 0,003086 ith: E is equal P2O5 with NaOH solution, g / mL; N is the normality of NaOH solution; Is equal to 0.003086 P2O5 1N NaOH, g / mL. NOTE 66 The value of the solution is based on the assumption that the phosphorus in cement precipitated as ammonium fosfomolibdat (2 (NH4)3PO4, 12 Moo3) and precipitate reacts with NaOH solution: 2 (NH4)3 PO4, 12MoO3 NaOH + 46 = 2 (NH4)2 HPO4 + (NH4) 2 Moo4 Na2MoO4 + 23 + 22 H2O. 0.003086 Figures obtained by dividing the molecular weight of P2O5 (141.96) with a 46 mm (46 is the amount of NaOH in the equation) and the 1000 (number of milliliters in 1 liter). Since the actual composition of the sediment is affected by the deposition conditions, by It is therefore important to pay attention to the order of procedure as it has been carefully described. 5）Sodium nitrite (NaNO2 50 g / L) （6）Standard solution, sulfuric acid (0.15 N) Dilute 4.0 mL H2SO4 to 1 L with fresh cold water bring to a boil. Standardise against standard solution of NaOH. Set the concentration ratio H2SO4 standard solution to volume by dividing the volume of NaOH solution by volume H2SO4 solution used in the titration. 3）procedure (1) Weigh (1-3) gram sample (NOTE 67) and 10 g of NH4NO3 into a glass chemistry 150 mL. Stir the mixture, add 10 mL HNO3, and stir quickly, with using a flat tipped rod to destroy clumps cement, cement decomposes to perfect and viscous gel of silica (SiO2) broke. Glass cover with a watch glass, place it over a water bath or plate heating at a temperature of approximately 100 ° C

for (15-20) minutes, and stir contents occasionally during heating. Add 20 ml of hot water into the beaker and stir the contents. If the cement contains high levels of manganese which is quite visible presence of residues red or brown, add a few milliliters of NaNO2 (50 g / L) to dissolve the residue. Boil the contents of the beaker until all nitrous fumes out. This procedure must be carried out in no more than 5 minutes, and the water should be added to replace the missing parts due to evaporation. Filter, using porous filter paper medium, into the beaker 400 mL under vacuum and the platinum cone to hold the filter paper Wash residual SiO2 with hot water until the volume of filtrate and water washings approximately 150 mL. NOTE 67 The number of samples and reagents are used depending on the level phosphorus in cement. The minimum amount required when the cement contains 0.5% P2O5 or greater. The maximum number is required if the P2O5 content determined is 0.1% or less. （2）Heat the solution at ambient temperature (69-71) ° C, remove from the heat source, and immediately add (50100) mL of ammonium molybdate. Stir the solution vigorously for 5 minutes, wash the inner side of the beaker with a cold solution of KNO3 (10 g / L), cover the beaker with a watch glass and let stand for 2 hours. Use suction, filter sediment (NOTE 68) solution by decantation interfere as little as possible precipitate. Stir the precipitate in a beaker with a stream of cold solution KNO3, decantation liquid, then wash the precipitate in the filter. Rub stirring rod and beaker with policemen, wash and pour contents above the filter. Wash the precipitate until free acid (NOTE 69), let each time adding inhaled perfect wash solution before subsequent additions. NOTE 68 filter paper filter can be ed on a porous medium with platinum cone or small hirsch funnel using filter paper cut suit and a thin layer of paper pulp or asbestos slurry was washed acid-free. Screening should be done with caution that has been washed free acid. Screening should be done with caution to avoid the loss of sediment. Filters should be really precise, and exploitation must be done before filtration and maintain until the washing is complete. NOTE 69 It is estimated about 10 washes. Test water washing to 10 with drops of indicator and a half drops phenophtalein standard solution of NaOH. If pink color appears and looks at least 5 minutes, the precipitate true acid-free, if not washing should be continued. (3) Remove the filter and precipitate into the beaker used for deposition, use a small piece of damp paper to clean funnel and lift sections of sediment may have on the funnel. Add 20 mL of cold water free of CO2 into the beaker and destroy filter paper with a policeman who used to scrub the

beaker. Add 0.3 N NaOH excess, stir the contents of the beaker until spotting yellow color disappeared, policeman and wall wash beaker with 50 mL of CO2-free cold water, and add 2 drops of neutral indicator phenolphatalein. Treat the solution with 0.15 N H2SO4 solution, in a measurable amount, enough to remove the pink color perfectly. Refine titration with NaOH solution until slightly pink survived for at least 5 minutes. 4) blank Create a blank determination, follow the procedures and reagents of the same amount, correction of the results obtained in the analysis. 5) Calculation Calculate the percentage of P2O5 to the accuracy of 0.01 as follows: ％P2O5= [E（V1-V2R）/ S]×100 with: E is equal P2O5 against NaOH solution, g / L; V1 is the milliliters of NaOH solution used; V2 is used milliliters of H2SO4; R is the ratio of the strength of the NaOH solution of H2SO4; S is gram sample used. 7.1.4.5 Mangan oxide 1) Summary of test method In this test method, manganese oxide defined by volumetric titration by solution of potassium permanganate. 2) Reagent (1) standard solution of potassium permanganate (0.18 N) Prepare a solution of potassium permanganate (KMnO4) and Standardise as described in clause 7.1.3.9.2.) (2), except for manganese oxide (Mn2O3) equality solution was calculated to equal the potassium oxide (CaO). Calculate Mn2O equality in solution as follows: E = (B x 0,3534) / A

with: E is equal to the solution of KMnO4 Mn2O3, g / mL; B is a gram Na2C2O4 used; A milliliter of solution is needed in KMnO4 titration Na2C2O4; 0.3534 is the ratio of molecules of 3Mn2O3 against 10 Na2C2O4. (2) Powder Zinc Oxide (ZnO) 3) Procedure (1) Place the 2 gram sample in a 250 mL beaker and add about 50 mL of water. Stir the mixture until there is a suspension and then add 15 ml of HCl. Heat the mixture gently to form a solution as perfect as possible. Add 5 mL HNO3 and 50 mL of water to the solution and simmer until most of the chlorine out. If necessary, add hot water to maintain the volume of ± 100 mL. Stop boiling and add ZnO powder into the solution until free acid. Add (3-5) g excess ZnO powder into the solution and bring to a boil for several minutes. (2) Without filtration, and the solution is maintained while still heated (90-100)° C by heating intermittently or continuously, titration with a solution 0.18 N KMnO4 standard, up to the addition of 1 drop of KMnO4 cause color pink is not lost anymore. Nearing the end point of the titration, let the sediment is slightly down, and observe the color coating solution from the side of a beaker. 4) blank Create a blank determination, quoting procedures and some of the same reagents and correction of the results obtained in the analysis. 5) Calculation Calculate the percentage of accuracy Mn2O3 to 0.01 as follows: % Mn2O3 = E V x 50 with: E is equal Mn2O3 with KMnO4 solution, g / mL; V is milliliters of KMnO4 solution used; 50 is 100 divided by the weight of sample used (2 grams).

7.1.4.6 Calcium oxide-free 1) Summary of test method This test method is a quick test to determine the free calcium oxide in fresh slag. If used for cement or slag that has a long, keep in mind the possibility of presence of calcium hydroxide, because this method does not distinguish between free CaO and Ca(OH)2 are free. Two test methods are provided. First, the alternative test method A is a modified procedure Franke which free lime titrated with perchloric acid aqueous solution after solution is the solvent ethyl asetosdetat-isobutyl alcohol. Second, an alternative test method B is the titration of ammonium acetate-alcohol glycerol to free lime with Sr (NO3)2 as a promoter. 2) The test method modifications Franke (alternative test method A) (1) Equipment a) Equipment reflux Consisting of erlenmeyer flask with a flat bottom short necked, capacity 250 mL. Reflux condenser water berpendinginan a minimum length of 300 mm. Pumpkin and reflux condenser connected with ground glass. Must be equipped with a reflux condenser tubes containing absorbent hair, such as silica gel, and materials to separate CO2, such as askarit. Absorber tube fitted with a rubber bagiah made up of reflux column. b) Burette Capacity of 10 mL and scale must not be greater than 0.05 mL. c) vacuum filter equipment. Consists of cup size No. Gooch. 3, a section 25 mL capacity filter paper placed inside the suit, size 21 mm, Walter cup holder, suction 500 mL flask and vacuum source vacuum. The cup half filled with compacted pulp. d) Grain cup boiling stones (2) the necessary solvents a) Solvent-isobutyl ethyl alcohol asetoasetat Three parts by volume of ethyl asetoasetat and 20 parts by volume of isobutyl alcohol. b) thymol blue indicator Dissolve 0.1 grams of powdered thymol blue indicator into 100 mL isobutyl alcohol. c) standard solution of perchloric acid

Solution of 22 mL of perchloric acid (70-72)% to 1 liter with isobutyl alcohol. Standardise this solution are as follows: 0.1000 gram Ignition primary raw calcium carbonate in krusibel temperatures (900 - 1000)oC. Refrigerate krusibel and its contents in a desiccator and weigh to the nearest 0.0001 grams to the weight remains. Perform weighing quickly to prevent water absorption and CO2. Move immediately CaO without grinding to a clean erlenmeyer flask and dried, and weighed again to the nearest empty krusibel 0.0001 gram, to determine the amount of CaO added. Then follow the procedures beginning with "Add 70 mL ethyl-isobutyl asetoasetat alcohol etc. "of items 7.1.4.6.2). (3). a). Calculate equality CaO against standard perchloric acid solution in grams per milliliter by dividing the weight of CaO used by volume perchloric acid required for titration. (3) Procedures a) Weigh 1.000 gram sample has been smoothed (NOTE 71) and transfer to a 250 mL erlenmeyer flask dry and clean. Add four to five cups boiling stones. Add 70 mL of solvent ethyl asetoasetat-isobutyl alcohol was prepared. Swirl the flask until the sample is dispersed. NOTE 71 Accuracy smoothing example is very important to liberation of free lime grains are often trapped in crystals tricalcium silicate in the cement. However, with the air sample should be kept as small as possible to avoid carbonation of free lime. Specifically, breathing directly into the sample should be avoided. examples have smooth enough to easily sieve no. 200 (75 μm) but not filtering is recommended. If the sample is not tested immediately, should be stored in an airtight container for avoid unnecessary with the air. b) Connect the flask with a reflux condenser and a treat to sample boil. Reflux for 15 minutes. c) Separate the pumpkin condensers, stoppers, and cool immediately to room temperature. d) Filter and solution examples using vacuum equipment. Wash pumpkin and residues gradually (10-15) mL with isobutyl alcohol up to a total volume of 50 mL wash solution. e) Add 12 drops of thymol blue indicator to the filtrate and titrate with 0.2 N perchloric acid until the color changes clearly. (4) Calculation Calculate the percentage of free calcium oxide with 0.1% accuracy:

% CaO free = with: E is the equality of CaO against perchloric acid, g / mL; V is milliliters of perchloric acid solution required by the sample; W is the weight of sample, grams. 3) rapid test methods Sr (NO3) 2 (alternative test method B) (1) Reagent a) standard solution of ammonium acetate (1 mL = 0.005 g CaO) Prepare a standard solution of ammonium acetate (NH4C2H3O2) by dissolving 16 grams of ammonium acetate (which has been previously stored in a desiccator) in 1 liter of ethanol in a closed botot dry and clean. Standardise this solution by the same procedure as in item 7.1.4.6.3.) (2). A) unless the next use as a substitute for example, ignition up to ± 0.1 gram fixed weight of CaCO3 with platinum krusible temperature (900-1000)oC. Cool in a desiccator and weigh its contents to the nearest 0.0001 gram. Perform weighing quickly to prevent water absorption and CO2. Immediately move CaO without mashed into a 250 mL boiling flask (glyserin solvent-containing ethanol and Sr (NO3)2, and weigh it again krusibel blank to determine the weight to the nearest 0.0001 gram CaO. Proceed in accordance with Section 7.1.4.6.3). (2). A) and 7.1.4.6.3). (2). B). Calculate equality CaO against ammonium acetate in grams per milliliter by dividing the weight of CaO used by volume solution needed. b) Indicators phenoltphalein Dissolve 1.0 grams phenolpthalein in 100 mL of ethanol (formula 2 B) c) Solvent glycerol - ethanol (1 + 2) Mix 1 part glycerin volume with 2 parts by volume of ethanol (formula 2 B). For each liter of this solution, add 2.0 mL of indicator solution phenolphthalein. NOTE 72 Ethanol has didenaturalisasi according to the formula 2 B (99.5% ethanol and 0.5% Benzol) is better but can be replaced with reagent grade isopropyl alcohol. d) Strosium nitrate Sr (NO3)2, reagent grade. (2) Procedure a) Remove 60 mL of glycerin-ethanol solvent into the flat bottom boiling flask 250 mL, clean and dry. Add 2 grams of anhydrous strontium nitrate (Sr (NO3) 2), and set the solvent to slightly alkaline by dropwise addition

of a solution NaOH solution and fresh in alcohol to form a red tinge young. Weigh 1.000 gram sample has been smoothed (NOTE 72) into the pumpkin, insert magnetic stir bar, and immediately connect with condenser cooling water (wearing glasses liaison sized 24/40). Boil the solution in the flask on the hot plate magnetic stirred for 20 minutes at moderate stirring. b) Remove the condenser and filter the contents of flask with polypropylene Buchner funnel under vacuum, use a 250 mL flask has the form tube to filter. Treat the filtrate to boiling and immediately titrate with a standard solution ammonium acetate to the colorless endpoint. (3) Calculation Calculate the percentage of free calcium oxide with accuracy of 0.1% as follows: % CaO free = EV x 100 with: E is equal to the solution of ammonium acetate CaO, g / mL; V is milliliters of a solution of ammonium acetate required by the sample.

7.2 Physical Test Methods 7.2.1 ing Materials and Devices 7.2.1.1 ing Materials 1) Room temperature testing set to (23 ± 1.7) °C, while the humidity chamber relative moisture test laboratory not less than 50%. 2) The definition of humid chamber is a room with a relative humidity of about 95% moisture. 3) If in testing used the water, then the water is distilled water. 4) The definition of cold water is the water having a temperature chamber. 5) Measurement of the amount of water is done with a measuring cup that has distribution of the size scale of 1 ml. 6) Weighing with accuracy to 0.01 grams should be done with scales with the highest capacity of 500 grams. Weighing with accuracy to 10 grams should be done with scales with the highest capacity of 5000 grams. 7.2.1.2 Devices 1) Standard sieve size of 150 um (No. 100) and 850 um (No. 20)

Wire netting for standard sieve shall be made of brass, bronze or suitable wire. Wire firmly attached to the frame with a depth of 50 mm from the top order. The connection between the frames with wire netting should be filled with solder to prevent the cement lagged in the connection. Filter frame should be round with Ø 203mm equipped with pan and its cover. 2) Scales 3) Analytic scales have a capacity of not more than 200 grams with accuracy of 0.0001 or scales with a constant load and can be read directly. 4) Scales should be able to re-reading with differentiation no more than 0.0002 grams and shall have accuracy to 0.0002 gram. Scales with direct reading should have sensitivity no more than 0.0001 gram. Conventional scales with 2 pans should have a maximum of difference 0.0003 gram if the weighing is done by changing pan. 5) Weights.

Weights should be checked at least once a year or re-adjusted if necessary with the tolerance are allowed for class III. For this purpose, each laboratory must be able to maintain the accuracy of or should have standard weights from 50 g to 10 mg in accordance with the minimum specifications of class III and must calibrate. 6) Brush.

Bristle brush limp cleaning is necessary for the purposes of cleaning 150 um sieve (no. 100). 7.2.2 Fineness Testing Using Blaine And Turbidimeter 7.2.2.1 Using Blaine Portland cement fineness testing using Blaine reference to ASTM C 204-00, Standard test method for fineness of hydraulic cement by air permeability apparatus. Testing with Blaine aimed at determining fineness stated in the specific surface area of portland cement, calculated as the sum total surface area cm2/gram, or m2/kg portland cement. 1) Devices 1) Blaine Blaine basically consists of a device that attracted a number of air through a base of portland cement prepared with a certain porosity, is a function of particle size and determine the flow rate of air through base. This tool is shown in Figure 3 and consists of the following sections: a.

Permeability cell

Permeability cell consists of a rigid cylinder with an inside diameter (12.70 ± 0.10) mm made of austenitic stainless steel. 1. The inside of the cell should be fine (fineness of 0.81 um). The upper part of the cell must be perpendicular to the main axis of the cell. The bottom of the cell must be able to form an airtight connection with the upper end of the manometer, so that no air leaks between the areas. Permeability cell consists of a rigid cylinder with an inside diameter (12.70 ± 0.10) mm made of austenitic stainless steel. 2. Holder (ledge) has width (0,5-1,0) mm is part of the cell that sticks firmly in the cell, at a distance of

(55 ± 10) mm, from the top of the cell to hold the metal plate with holes. The top of the permeability of the cell must be fitted to the outside of the stand, for easy retrieval of cells from the manometer. b.

Disc 1. The disc is made of rust-resistant steel with a thickness of (0.9 ± 0.1) mm holes as many (30-40) holes with Ø 1 mm and spread evenly. 2. The plate should match the interior of the cell, the center of one side of the plate should be marked or scratches that can be read, so testers are always out to put a hand at the bottom if you put it in the cell.

c.

Plunger 1. Plunger is made from austenitic stainless steel to be precise entry into the cell with a tolerance of no more than 0.1 mm. 2. The bottom of the plunger should really be flat and perpendicular to the main axis. 3. Plunger must be equipped with an air vent in the form of a flat section with width (3.0 ± 0.3) mm on one side. 4. The highlight of the plunger is fitted to the outside of the stand, so that when the plunger is inserted into the cell and the cell that stand in with the top of the cell then the distance between the base of the plunger to the top of the plate should be (15 ± 1) mm.

d.

Filter paper should have a medium air flow resistance, circular with a flat edge and has a diameter equal to the diameter of the inside of the cell.

e.

Manometer Manometer made of glass U-shaped tube with an outer diameter of 9 mm, as shown in Figure 3. The upper part of one arm should be able to form an airtight connection with the cell permeability. arm manometer that connected to the cell permeability should have a line mark that circles the tube (125-145)

mm below the top of the disposal, as well as other lines within (15 ± 1) mm, (70 ± 1) mm , and (110 ± 1) mm above the line. Disposal should be placed (250-305) mm above the base manometer, used to discharge air at manometer arm connected to the cell permeability. Manometer should be equipped with a positive airtight valve or clamp that is located not more than 50 mm from the manometer arm. Manometer should be sturdy installed, so both arms straight.

Figure 3. Blaine

f.

Manometer fluid

Manometer should be filled to middle of the line of the tube with a liquid that does not easily evaporate, not hygroscopic, has a low viscosity and density, such as dibutyl ptalat (dibutyl 1.2 benzene dicarboxylic) or light mineral oil. g.

Timers Timers must be equipped with start and stop buttons, and should be read up to 0.5 seconds or less.

h.

For the time range from 0 seconds to 60 seconds. Timer shall have a maximum accuracy of 0.5 seconds, and time span should be second, with a maximum of 1% accuracy.

2) Other devices. a.

Small funnel accordingly.

b. Small fluffy brush (no. 7). c.

Scales cup

d. Analytic scales according to the specifications. 2) Calibration 1) Standard cement sample For calibration blaine should use standard cement from NIST, Standard Reference Material No.. 114. Cement sample shall be adjusted first to the room temperature. 2) Determination of the volume of cement layer (bed) Determination of the volume of cement layer is done by moving the mercury as follows: a. Place two pieces of filter paper circle inside the cell diameter slightly smaller than a cell, until all the filter paper flat on a metal plate and fill the cell with mercury, ACS quality or better, to eliminate air bubbles attached to the cell wall. Use tongs (tongs) when carrying cells. If the cells of the material that will be amalgam with mercury, the inside of the cell should be given a protective coating a very thin oil before adding mercury. Then fill the cell with mercury. Flatten with the top surface of the cell using a glass plate that is emphasized is slowly on the surface of the mercury, to be sure there are no air bubbles or voids between the surface of the mercury and the glass plate. Remove mercury from inside cells, weigh and record the weight.

Remove one of the filter paper from cell, and then on the filter paper is left filled with one a layer of cement is made by inserting less than 2.80 grams of cement (no cement standards) and place the filter paper was issued earlier in the cement. Then press the layer of cement with plunger until the neck of plunger with the cell surface (NOTE 73) NOTE 73 Preparation of cement paste should be solid. If it is too loose or cement cannot be reduced to the base with the desired volume, then in this case adjust the amount of cement used in the experiment. The empty room on top of a layer of cement then filled with mercury, and the flattened surface like the way mentioned above. Remove this mercury, then weigh and record the weight. b. Calculate the volume of portland cement pedestal accuracy of 0.005 cm3 up with the formula: ………………………… (1) with : V

is the volume of portland cement, cm3

Wa

is the weight mercury required to fill the cell with no portland cement layer, gram

Wb

is the weight mercury required to fill the empty part of the cell occupied by a layer of Portland cement, gram

D

is the density of mercury at the test temperature, gram/cm3

c. Determination of the volume of portland cement layer has to be done at least twice, and for each separate

determination compacted cement layer. Price volume cement layer used for the average calculation should come from two prices with the determination of a maximum difference of ± 0.005 cm3. Ambient temperature around the cell should be recorded at the beginning and end of the experiment. 3) Preparation of sample Enter a standard semen sample from vials into a bottle with volume was about 120 cm 3, shake vigorously for two minutes to break the clumps. Leave the bottle in an up and covered for two minutes, then open the lid and stir gently to flatten the particles have to be homogeneous. 4) Weight standard sample Weight standard sample for calibration should be taken in such a way as to obtain a standard cement layer having porosity of 0.500 ± 0.005 and was calculated using the formula: W = ρ v (1 – e ) ……………..……..(2)

with : W

is a standard example of the required weight, gram;

ρ

is a portland cement sample density values used were 3.15 mg/m3 or 3.15 g/cm3;

v

volume of cement layer standards prescribed in the manner described in clause 7.2.2.1.2.) (2), cm3;

e

is the porosity of the cement layer of the desired standard (0.500 ± 0.005), (NOTE 74).

NOTE 74 Porosity is the ratio of the volume of the cavity with the overall volume of the cement layer. 5) Preparation of the cement layer Place the metal disc at the base of the cell, put a paper filter on top of the metal plate and press down with a trunk diameter slightly smaller than the diameter of the cell, so that the plate and filter paper are in the right position. Weigh the amount of cement with accuracy to 0.001 gram weight determined in accordance with the calculation above, in point 7.2.2.1.2). (4), and enter into the cell. Slowly knock the outer cell wall layer of cement to smooth it. Put a piece of filter paper on top of a layer of cement and press the plunger until the plunger neck with the surface of cells. Pull the plunger slightly upward, turn 90 degrees, then slowly press the plunger is pulled out of the cell. 6) Determination of the permeability of the layer of cement Every time determining permeability layer of cement should be used new filter paper. a. Connect the permeability cell of the manometer tube with airtight connections in such a way that does not interfere with layer of cement that had been prepared earlier (NOTE 75) NOTE 75 Apply a little lubricant on the valve that connecting manometer, one of the manometer arm closed, slightly open and then close again. If there a constant pressure drop indicates a leak in the system. b. Slowly remove existing air in one tube manometer until the manometer liquid reaches the top line mark, then close the valve tightly. c. Run the timer when the liquid reaches the bottom miniskus mark the second line from the top, stop when the liquid reaches the bottom miniskus third dash. d. Record the observed period (seconds) and test temperature (oC)

e. In blaine calibrating, at least do three times the timing flow, and each time using a different standard cement layer. Calibration should be done by testers who did the fineness test (NOTE 76).

NOTE 76 Sample cleared from hairbrush and can be reused, as long as it is kept in a dry state, and all the tests carried out within 4 hours after the sample is opened. 7) Recalibration Device must be recalibrated if blaine (NOTE 77): a. At a certain time period, which is necessary for the correction of possibility worn-out plunger or permeability cells. b. Loss of fluid in the manometer. c. If need types or quality of different filter paper. NOTE 77 Recommended setting up and using a secondary standard that is used as a standard to calibrate the tool between the fineness of calibration with standard semen sample. 3) Procedure 1) Temperature semen sample tested should be the same as the temperature of the room at the time of testing 2) Weight sample to be tested must be equal to the weight of cement standards for calibration as described in paragraph 7.2.2.1.2.) (4), except when determining the fineness of cement type III or other more subtle type, the weight of it is very large so that the pressure with the thumb cannot cause plunger neck with a peak cell. Sample weight is required to be such that a layer of semen samples have porosity 0.005 ± 0.500. 3) Preparation of cement layers Preparation of cement in accordance with Section 7.2.2.1.2). (2) 4) Permeability testing Permeability testing in accordance with Section 7.2.2.1.2). (6) except in the determination of flow time only once. 4) Specific face area calculating 1) Specific face area is calculated by the following formulas: ……………………………………………………. (3)

S=

……………………………………………………. (4)

S=

……………………………………………………. (5)

S=

……………………………………………………. (6)

S=

……………………………………….…………… (7)

S=

………………………………………………….... (8)

with : S

is the specific surface area of the cement sample tested, cm2/gram;

Ss

is the specific surface area of the standard semen that used in the calibration, cm2/gram;

T

is the time span of the pressure drop in the manometer for portland cement sample tested, second;

T2

is the time span of the pressure drop in the manometer for standard semen used in the calibration, second;

η

is the viscosity of air at temperature testing semen samples tested, poise;

ηs

is is the viscosity of air at temperature testing standard semen used for calibration, poise;

e

is the porosity of layers of cement sample tested;

es

is the porosity of layers standard semen used in the calibration standards;

ρ

is the density of the standard semen samples tested (set value 3.15);

ρs

is the density of semen samples used in the calibration standard (3.15 mg/m3 or 3.15 considered gram/cm3);

b

is a constant (for portland cement 0.9).

NOTE 78 Value η, e3 and T, respectively obtained from Table 6 and Table 7. 1. Equation (3) and equation (4) is used to calculate the fineness of portland cement sample was compacted to

achieve the same porosity with standard semen sample used for calibration. Equation (3) is used when the maximum temperature is different experiments of 3oC temperature calibration experiments and equations (4) if the temperatures differ by more than 3oC experiments with temperature calibration experiments.

2. Equation (5) and equation (6) is used to calculate the fineness of portland cement sample was compacted to achieve a different porosity with standard semen sample used for calibration. Equation (5) is used when the difference in the maximum temperature in the calibration experiments 3oC and equation (6) is used digunaakn when the temperature calibration experiments differed by more than 3oC 3. Equation (7) and equation (8) is used to calculate the subtlety materials other than portland cement.

Equation (7) is used when the temperature is different experiments ± 3oC of temperature calibration experiments and equation (8) is used when temperatures differ by more than 3oC experiments with temperature calibration experiments. 2) To calculate the specific surface area in units of m2/kg, multiply the surface area by a factor of 0.1 in cm2/gram 3) Round price in cm2/gram to tithe while m2/kg rounded nearest closest unity

example: 3447 cm2/gram rounded to 3450 cm2/gram or 345 m2/kg 5) Report 1) For cement and cement-based material, the determination of just once. 2) For any material with high fineness with the lapse of time, report the average fineness of the two permeability

testing to record the difference is not more than 2%. If the difference is outside the provisions above, repeated testing is done to comply with the price difference. Table 9. Mercury density, air viscosity (ηs) and ηs at a certain temperature Room Temp.

Mercury Density

Air Viscosity, (ηs)

(oC)

(g/cm3)

poise

16

13.56

0.0001788

0.01337

18

13.56

0.0001798

0.01341

20

13.55

0.0001808

0.01345

22

13.54

0.0001818

0.01348

24

13.54

0.0001828

0.01352

26

13.53

0.0001837

0.01355

28

13.53

0.0001847

0.01359

ηs

30

13.52

0.0001857

0.01363

32

13.52

0.0001867

0.01366

34

13.51

0.0001876

0.01370

Table 10. The values of porosity cement layer Porosity Of Layer Cement

e3

E 0,495

0,348

0,496

0,349

0,497

0,350

0,498

0,351

0,499

0,352

0,500

0,354

0,501

0,355

0,502

0,356

0,503

0,357

0,504

0,358

0,505

0,359

0,506

0,360

0,507

0,361

0,508

0,362

0,509

0,363

0,510

0,364

0,525

0,380

0,526

0,381

0,527

0,383

0,528

0,384

0,529

0,385

0,530

0,386

0,531

0,387

0,532

0,388

0,533

0,389

0,534

0,390

0,535

0,391

Table 11. The range of air flow time

7.2.2.2 With Turbidimeter Fineness testing by the turbidimeter referenced to ASTM C 115-96a Standard test method for Fineness of portland cement by the turbidimeter. Test method for fineness of portland cement by using turbidimeter. 1) Devices 1)

Standard Device

Turbidimeter Wagner is comprised of a light source that is maintained at fixed intensity and arranged so that a parallel beam of light ing through a suspension of cement were tested and the electrical photo-sensitive plate. The electric current generated by the cell was measured by a micrometer and reading is indicated a measure of the turbidity of the suspension. The main estimates indicate that turbidity is a transitional measure the surface area of the suspended semen sample. Device shall consist of specific parts described in paragraph (2) to point (7) and have been prepared in accordance with a complete design and dimension requirements as in Figure 4 to Figure 7 and Table 12, except for the wooden or metal.

Figure 4a. Turbidimeter looks ahead with open doors

Figure 4b. Turbidimeter looks ahead with open doors

Figure 5. Rear Turbidimeter

Figure 6. Buret Time

Figure 8. Electrical system Turbidimeter

Table 12. Dimension Turbidimeter Device

Image Information

Dimension (mm)

A

445

B

438

C

381

D

105

E

3.0

F

28.6

G

85.7

H

33.3

I

102

J

39.7

K

55.6

L

65.1

M

28.6

N

3.0

O

51

P

51

Q

3.0

R

61.1

S

69.8

T

51

U

22.2

V

34.9

W

13

X

38

Y

15.9

Z

38 ± 0.75

AA

51 ± 2.5

AB

267

AC

…

AD

…

AE

39.7

AF

55.6

AG

66.7

AH

2.3

AI

23.6

AJ

1.38A

AK

cmA

NOTE A

That number is the real number that is part of the goal and the numbers connecting parts; consequently do not relate to the title of the column.

2)

Turbidimeter

Mounted in a wooden box or metal fittings as follows: a. The light source The light source in Figure 4b consists of an electric lamp with a filament that is concentrated between 3-6 candela operated by a source with constant emf. Lights should be installed firmly in the socket. Metal parabolic reflectors are clean and shiny should be strong paired opposite the light, focused in such a way that roughly parallel beam of light will through the sedimentation tank and the photoelectric cell. Light intensity should be set using two reostat approximately 6 ohms and 30 ohms and reostat must have certain characteristics which are uniformly changes in light intensity is obtained through the range full of resistors. Reostat should be installed in parallel with each other and in series with the lamp. b. Heat absorbing device Light must through a heat absorbing device before entering the sedimentation tank during the heat radiation from the light beam to be absorbed, the device can be:

a) cells or water; b) special heat absorbing glass filter heat sink. Water cells should be made of brass pipe without a seam that has an outer diameter of 76 mm, a wall thickness of 3 mm and a length of 102 mm with glass windows were glued end. Cells must have a hole to fill distilled water. The hole should be closed with plugs of metal. Cell on when placed on the stand who could move to have good cover at a position above or below. Heat absorbing device must be structured in such a way that all the beams of light from the lamp into the sedimentation tank through a heat absorbing device. c. Inhibitors Glass to be provided for the reduction of light to reduce light intensity from 100 µA to 20 µA to 30 µA. Light intensity should be reduced uniformly throughout the cell that are ed by the light during testing. Inhibitors must be installed in a frame can be swung out of the path of light by using a holder. d. Sedimentation tank Sedimentation tank shall be: a) Glass plates (5-6) mm or boro silicate glass are cemented or glued together to form a square tank, or; b) Printed glass tank which has a wall thickness of about 5 mm with a flat surface. The dimensions of the tank should have a length of 51 mm width 38 mm and height of 203 mm. Variations are allowed for the tank dimensions are length and width ± 2.5 mm ± 0.76 mm. Face of tank 51 mm should have the same distance of 0.25 mm at all points. Signs must be placed on the side of the tank to indicate the contents of the volume of 335 ml which is the limit of the tank during the test. The tank is filled with clear kerosene up to the mark and placed on a beam of light turbidimeter, will produce a uniform micrometer reading ± 0.1 µA, to all parts of the tank that can be used. e. Photoelectric cell Device used to measure the light intensity must be electrically sensitive photo cells are linked directly with the micrometer. Cover with a horizontal slot with 13 mm height, 35 mm width should be mounted on an electric photo cell. The front of the cover should be (25 ± 1) mm at the front face of the cell. Cell face should be parallel to the face of the tank with a distance of 0.05 mm. f. Protector Protective metal using the high slot 16 mm, width 38 mm. Should be placed between the heat absorbing devices and the sedimentation tank.

Appendix A (Informative) Sample record form chloride determination Table A.1 Sample form determination of the equivalence point in the determination of chloride column 1 AgNO3, mL 1,60

column 2 Potential, mV 125,3

Column 3 A ΔmV

Column 4 2 B Δ mV

1,80

119,5

5,8

1,4

2,00

112,3

7,2

1,3

2,20

103,8

8,5

1,3

2,40

94,0

9,8

0,6

2,60

84,8

9,2

2,3

2,80

77,9

6,9

0,8

3,00

71,8

6,1

1,3

3,20

67,0

4,8

Appendix B (Informative） Examples of qualifying results Table B.1 initial bonding time Binding early Cement

Series

A

1

A method 95

Unit in minute Binding early difference average B method (spek. max 45) 105 …

A A Julat （Spek.30 Maks） Average B B B Julat （Spek.30 Maks） Average C C C Julat （Spek.30 Maks） Average

2 3

90 95 5

105 90 15

… … …

1 2 3

93,3 100 105 85 20

100 120 95 95 25

6,7 … … … …

1 2 3

96,7 155 155 145 10

103,3 170 160 155 15

6,7 … … … …

151,7

161,7

10,0

Table B.2 final bonding time Cement

Series

A A A Julat （Spek.30 Maks） Average B

1 2 3

1

Binding early

Binding early

A method 150 145 170 25

A method 150 150 125 25

Unit in minute difference average (spek. max 45) … … … …

155 185

141,7 180

13,3 …

B B Julat （Spek.30 Maks） Average C C C Julat （Spek.30 Maks） Average

2 3

1 2 3

200 185 15

180 155 25

… … …

190 235 240 240 5

171,7 225 220 215 10

18,3 … … … …

238,3

220

18,3

Appendix C (Informative) Stirring mechanical hydraulic cement paste and plastic consistency of mortar 1 The scope Practical ways include mechanical mixing of hydraulic cement pastes and consistency plastic from the mortar.

2 Purpose and use This method is intended for use on mechanical stirring on pasta and for testing hydraulic cement mortar. 3 Equipment 3.1 Purpose and use This method is intended for use on mechanical stirring on pasta and for testing hydraulic cement mortar. Mixing machine shall be equipped with spacer retainer as shown in Figure 12, which should be used to keep the distance between the bottom of the mixer the bottom of the bowl is not greater than 2.5 mm, but not less than 0.8 mm approximately equal to the diameter of Ottawa sand (20-30) when the bowl is in a position stirring. 3.2 Mixer Mixer should be easily dismantled pairs, made of stainless steel, and the design essentially as described in Figure 13. If in the position following the stirring of bowl shape is used, the shortest distance between the tip and the inner wall mixer bowl of ± 4.0 mm but not less than 0.8 mm. 3.2 Mixer Bowl Mixing bowls that can be assembled must have a nominal capacity 4.73 L. Meets dimensional and have as in Figure 14, and must be made of stainless steel. The bowl comes with parts that can be attached to either the mixing equipment with a strong position during mixing walks. Must be equipped with a lid made of non absorption and not damaged by cement. 3.3 Rake Rake should consist of a rubber blade half kapok equipped with handle ± 150 mm in length. Blade length ± 75 mm, width 50 mm and tapers to the side thin sections of ± 2 mm. 3.4 Other Tools Scales, weights, glass sizes other tools used in the measurement and preparation of ingredients before mixing mortar must meet appropriate requirements. 4 Temperature and humidity 4.1 One room, dry ingredients, mixing bowls and must be maintained between (20 to 27.5)oC. Mixing water temperature should be (23 ± 1.7)oC. 4.2 Humidity laboratory at least 50%. Temperature and humidity in accordance with theclause 7.3.1.

5 Ingredients, proportions and consistency 5.1 Requirements Materials, proportions and consistency as well as the amount of material must meet the requirements contained in the particular method in which a paste or mortar prepared. 5.2 Procedure stirring pasta 5.2.1 Install a dry mixer and bowl with mixer on positioning stirring. Then enter the ingredients for mixing into one bowl as follows: a) enter all the water into the mixing bowl; b) add the cement into the water and let sit for 30 seconds, for the absorption of water; c) run the engine at low speed stirrer 140 rpm ± 5 rpm for 30 seconds. 5.2.2 Stop the mixer machine 15 seconds and during this time clear the inner walls in a bowl of pasta sticking. 5.2.3 Run the mixer at medium speed engines with rotation (285 ± 10) rpm and stir for 1 minute 5.3 Procedure mixing mortar 5.3.1 Install the stirrer and stirrer dry bowl mixer with stirring positions. Then enter the ingredients into a mixing time bowl as follows: a) enter the water in a mixing bowl; b) add the cement into the water, then run the machine agitator stirring at low speed 140 rpm ± 5 rpm for 30 seconds; c) add all the sand slowly in 30-second intervals, stirring in low speed 140 rpm ± 5 rpm. 5.3.2. Stop the mixer machine, replace the medium speed (285 ± 10) rpm, and stir for 30 seconds. 5.3.3. Stop the engine and allow the mortar mixer for 1.5 minutes. For 15 seconds first time intervals, immediately clean the mortar that attaches to the inner wall of the bowl, then cover the bowl. 5.3.4. Continue stirring for 1 minute late at medium speed (285 ± 10) rpm. 5.3.5. If necessary, at any time interval required stirring again, every mortar attached to the inner wall of the bowl should be cleaned with a rake before stirring re-done.

BIBLIOGRAFI ASTM C 150-02a, Standard Specification for Portland Cement BS 12-1996, Specification for portland cement