complete chemical analysis of portland cement

Cement chemical analysis

Item ................................................ .................................................. ...... 2

General ................................................ 1.................................................. .. 3

Sample............................................... 2.................................................. ... 4

Analysis............................................... 3 ............................................. 5

3.1 Determination of loss on ignition............................................ ......................... 5

3.2 Preparation of sample solution systems analysis.................................................. 5

3.3 Determination of silica............................................ ...................... 6

3.4 Determination of iron oxide ........................................... ................... 7

3.5 aluminum oxide, titanium dioxide Determination......................................... .. 9

3.6 Determination of calcium oxide ............................................. ...................... 11

3.7 Determination of magnesium oxide ............................................. ...................... 11

3.8 Determination of sulfide sulfur............................................ .................... 12

3.9 Determination of total sulfur............................................ ....................... 14

Sulfate Sulfur............................................ 3.10 ............... 17

Appendix A permissible error of measurement results

(Supplement)....................................... .... 19

Annotated... ............................................. 20

1 General

1.1 This standard applies to the expansion of cement and alunite using the standard

methods for other cement.

1.2 Determination of water refers to the use of distilled or deionized water. Reagent and

analysis procedures should be strictly in accordance with the provisions of this standard

method.

1.3 reagents should be analytical or superior grade pure reagents for calibration of

reagents, unless otherwise stated should be the benchmark reagents. On the determination

of the purity of water used and the reagent should be tested if in doubt.

1.4 Where the percent concentration of the reagent that is applied to 100 ml of solvent-

solute increase in the number of grams of preparation. The use of acid or ammonia, have

not traveled by state are concentrated acid concentration or concentrated ammonia.

1.5 with the analytical balance should not be less than four. Balance and weight should be

on a regular basis for examination. Used burette, volumetric flask, pipette should be

corrected.

1.6 When conducting chemical analysis, must make the determination of loss on ignition.

Various other blank test should be measured simultaneously, and the test results to be

corrected.

1.7 Analysis of results according to the percentage of samples that are reserved to the

determination of the second digit after the decimal point.

2 samples

Divided by the bulk sample after sample reduction, not less than 100 grams, fineness by

0.08 mm square hole sieve sieve shall not exceed 15%. Then quartering or splitter will

reduce the sample reduced to about 25 grams of milk agate mortar and then placed all

through the aperture in the ground to 0.08 mm square hole sieve, into a small sample

bottle, release the desiccators for analysis. The remaining samples as preserved as

backup.

3 Analyses

3.1 Determination of loss on ignition

Weigh sample of about 1.0 ± 0.1 g (accurate to 0.0001 grams), burning has been placed

in constant weight porcelain crucible. The crucible and the crucible placed on the inclined

cover, release the high-temperature furnace, the temperature gradually increased from the

low temperature; burning at 800 ℃ for 40 minutes. Remove the crucible, placed in the

desiccators to cool to room temperature and weigh. Repeat this operation (ignition every

30 minutes), until constant weight.

The percentage loss on ignition content (X1) calculated as follows:

G-G1

X1 = ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (1)

G

Where: G ─ ─ burning before the sample weight, g;

G1 ─ ─ the weight of sample after ignition, grams.

3.2 Preparation of sample solution systems analysis

3.2.1 Reagents

Sodium hydroxide

Hydrochloric acid

Hydrochloric acid (1:5): 5 to 1 volume of hydrochloric acid and water mixed volume.

Nitric acid.

3.2.2 Preparation

Weigh sample of about 0.50 ± 0.02 g (accurate to 0.0001 g), placed silver in the crucible.

Add 7-8 grams of sodium hydroxide, covered crucible lid (leave large gaps), has been

heated to 400 ℃ into the high-temperature furnace, continue to heat up to 650 ℃, and at

this temperature for 20 minutes. Remove the crucible, let cool, and has been placed in hot

water containing about 100 ml beaker. Covered glass dish, heat, until the melt extraction,

remove the crucible and the crucible wall of water washed. Then add 30 ml hydrochloric

acid once, stirring with a glass holding, so that the melt is completely dissolved. Amount

of hot hydrochloric acid (1:5) to the crucible wall and wash the crucible cover. Add 1 to 2

ml nitric acid and the solution heated to boiling. Subject to the clear and transparent

solution, the solution is cooled to room temperature, into 250 ml volumetric flask, dilute

to the mark with water, shake.

The sample solution for determination of silica, iron oxide, aluminum oxide, titanium

dioxide, calcium oxide and magnesium of the use of helium.

3.3 Determination of silica

3.3.1 Reagents

Nitric acid.

15% potassium fluoride solution:

15 g potassium fluoride (KF · 2H2O) dissolved in 50 ml of water, add 20 ml nitric

acid, diluted to 100 ml, add solid potassium chloride to saturation, place, 24 hours after

the fast The solution was filtered on filter paper plastic bottle and set aside.

Potassium chloride.

5% potassium chloride solution:

5 g of potassium chloride dissolved in 100 ml of water.

5% potassium chloride and ethanol solution:

5 g of potassium chloride dissolved in 50 ml of water, add 50 ml 95% ethanol,

and mix. ?

0.15N sodium hydroxide standard solution:

60 g sodium hydroxide dissolved in 10 liters of water, shake well, stored in a

belt stopper (with soda lime drying tube) rigid glass or plastic bottle.

Calibration method:

Weigh about 0.8 g of potassium hydrogen phthalate (accurate to 0.0001 g),

placed in 400 ml beaker, add about 150 ml of cold boiled new (the cold steel hydroxide to

phenol and phenol solution was slightly red) to dissolve. Then add 5-6 drops of

phenolphthalein indicator solution and titrate with standard sodium hydroxide solution to

reddish.

Standard solution of sodium hydroxide titer of silica calculated as follows:

G × 0.01502 × 1000

TSiO2 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (2)

V × 0.2042 Where: TSiO2 ─ ─ per milliliter of standard solution of sodium hydroxide is equivalent

to the number of milligrams of silicon dioxide;

G ─ ─ the weight of potassium hydrogen phthalate, g;

V ─ ─ titration, the volume of consumption of sodium hydroxide standard solution, ml;

0.01502 ─ dioxide equivalent per mg of grams;

0.2042 ─ equivalent per mg of potassium hydrogen phthalate grams.

3.3.2 Analysis Procedure

Article 3.2 of the standard drawing of the sample solution prepared in 50 ml into 300 ml

plastic cup, add 10 ml nitric acid, cooled to room temperature. Add 10 ml of 15%

potassium fluoride solution, holding plastic mixing, add potassium chloride to saturation.

Place 15-20 minutes to medium-speed filter paper filter. Plastic cups and precipitated

with 5% potassium chloride solution, washed 2 to 3 times. Together with the filter paper

placed in the original plastic sediment cup, along the cup by adding 10 ml of 5%

potassium chloride - ethanol solution and 10 drops of 1% phenolphthalein indicator

solution with 0.15N sodium hydroxide standard solution and in the end to make the acid,

filter paper and subsequently cleaned carefully stirred until the solution was red.

Then add 200 ml boiling water (with sodium hydroxide solution prior to phenol and

phenol was slightly red) to 0.15N sodium hydroxide standard solution titration to reddish.

Percentage of silica content (X2) calculated as follows:

TSiO2 · V × 5

X2 = ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (3)

G × 1000

Where: TSiO2 ─ ─ per milliliter of standard solution of sodium hydroxide is equivalent

to the number of milligrams of silicon dioxide;


5 ─ ─ all the points to take the sample solution and sample solution volume ratio;

G ─ ─ test weight, grams.

3.4 Determination of iron oxide

1.4.1 Test?

Ammonia (1:1):

The ammonia mixed with an equal volume of water.

Hydrochloric acid (1:1):

The hydrochloric acid mixed with an equal volume of water.

10% sulfosalicylic acid solution of sodium indicator,

10 g sulfosalicylic acid sodium dissolved in 100 ml of water.

Calcein - methyl thymol blue - phenolphthalein (hereinafter abbreviated CMP)

mixed indicator:

Weigh 1.0 g of calcein, 1.0 g methyl thymol blue and 0.2 g of phenolphthalein,

and 50 g in 105 ℃ dry mixture of potassium nitrate had small study, stored in a jar mill.

20% potassium hydroxide solution: 20 g of potassium hydroxide dissolved in 100 ml of

water.

Standard solution of calcium carbonate,

Weigh in 105 ~ 110 ℃ drying over 2 hours of calcium carbonate (high purity

reagents) about 0.8 grams (accurate to 0.0001 g), placed in 400 ml beaker, add about 100

ml of water, cover surface of the pan, along the cup dropping hydrochloric acid (1:1) to

all the dissolved calcium carbonate, heat to boil a few minutes. The solution was cooled

to room temperature, transferred into 250 ml volumetric flask, dilute to the mark with

water, shake.

Precision PH test paper: pH 0.5-5.0.

0,015 M disodium ethylene diamine tetra-acetic acid

(Hereinafter abbreviated EDTA)

Standard solution: Weigh 5.6 g EDTA placed in a beaker, add about 200 ml of water, heated to

dissolve, filter, dilute to 1 liter.

Calibration method:

draw 25 ml standard solution of calcium carbonate, releasing 400 ml beaker,

diluted to about 200 ml. Adding an appropriate amount of the CMP mixed indicator,

under the 71/92 mixing 20% potassium hydroxide solution to a green fluorescence, and

then over 2 to 3 ml with 0.015M EDTA standard solution drops away to the green and

red fluorescence disappears.

C×25 MFe2O3 C×25

TFe2O3 ＝ ─────×────── ＝ ──── ×0.7977 ⋯⋯⋯⋯⋯⋯（4） V 2MCaCO3 V

C×25 MAl2O3 C×25

TAl2O3 ＝ ───── ×────── ＝ ──── ×0.5094⋯⋯⋯⋯⋯⋯（5） V 2MCaCO3 V

C×25 MTiO2 C×25

TTiO2 ＝ ────×────── ＝ ──── ×0.7983⋯⋯⋯⋯⋯⋯⋯⋯（6） V MCaCO3 V

C×25 MCaO C×25

TCaO ＝ ────×────── ＝ ────×0.5603⋯⋯⋯⋯⋯⋯⋯⋯⋯（7） V MCaCO3 V

C×25 MMgO C×25

TMgO ＝ ────×────── ＝ ────×0.4027 ⋯⋯⋯⋯⋯⋯⋯⋯⋯（8） V MCaCO3 V

Where:

T Fe2O3 ─ ─ ─ number of milligrams of iron oxide equivalent per

milliliter of standard solution of EDTA ;

T Al2O3 ─ ── number of milligrams of aluminum oxide equivalent per

milliliter of standard solution of EDTA

T TiO2 ─ ─ number of milligrams of titanium oxide equivalent per


T CaO ─ ─ number of milligrams of calcium oxide equivalent per


T MgO ─ ─ number of milligrams of magnesium oxide equivalent per


C ─ ─ , the number of milligrams per milliliter of standard solution containing calcium

carbonate, calcium carbonate;

25 ─ ─ the volume of standard solution of calcium carbonate, ml;

V ─ ─ calibration standard solution of EDTA consumption volume, ml;

M Fe2O3 ─ ─ molecular weight of iron oxide;

M Al2O3 ─ ─ three ammoniated molecular weight of aluminum;

M TiO2 ─ ─ two ammoniated molecular weight of titanium;

M CaO ─ ─ molecular weight of calcium oxide;

M MgO ─ ─ molecular weight of magnesium oxide;

M CaCO3 ─ ─ molecular weight of calcium carbonate.


Article 3.2 of the sample solution prepared ,

take 50 ml into 300 ml beaker, diluted with water to about 100 ml. With ammonia (1:1)

solution adjusted to pH 1.8 ¯ 2.0 (the precise pH test paper test).

The solution heated to about 70 ℃.

Add 10 drops of 10% sulfosalicylic acid solution of sodium indicator to 0.015M EDTA

standard solution to bright yellow slow titration (end point when the solution temperature

should be about 60 ℃).

The percentage of iron oxide content (X3) calculated as follows:

TFe2O3 × V × 5

X3 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (9)

G × 1000

Where:

TFe2O3 ─ ─ number of milligrams of iron oxide equivalent per


V ─ ─ titration, the volume of EDTA standard solution consumed, ml;

5 ─ ─ sample solution volume ratio;

G ─ ─ sample weight, grams.

3.5 Aluminum oxide, Titanium dioxide determination

3.5.1 Reagents

0. 015M EDTA standard solution.

Ammonia (1:1).

Acetic acid a sodium acetate buffer solution (pH4.2):

33.9 g of anhydrous sodium acetate dissolved in water, add 80 ml glacial acetic

acid, then diluted with water to 1 liter shake (with precision pH meter or pH paper test).

0.2% PAN indicator solution:

0.2 g PAN (1 - (2 - pyridylazo) -2 - naphthol) dissolved in 100 ml ethanol.

5% mandelic acid solution:

5 g of acid-soluble bitter almonds in 100 ml of water, with ammonia (1:1), adjust

the pH to 3.5 or so (with a precision pH test paper test).

Precision pH test paper: PH 0.5 - 5.0.

0.015M copper sulfate standard solution:

3.7 g copper sulfate (CuS04.5H2O) dissolved in water, add 4-5 drops of sulfuric

acid (1:1), diluted to 1 liter shake.

EDTA standard solution and copper sulfate solution volume ratio of the calibration

standard; Burette slow release of 10-15 ml 0.015M EDTA standard solution in 400 ml beaker,

diluted to about 200 ml,

Add 15 ml acetic acid a sodium acetate buffer solution (pH4.2 ), heat to boiling. Remove

, cool,

add 5-6 drops of 0.2% PAN indicator solution to 0.015M standard solution of copper

sulfate titration to bright purple.

EDTA standard solution with concentration of copper sulfate standard solution volume

ratio (K) calculated as follows:

V1

K = ─ ─ ─ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (10)

V2

Where:

K ─ ─ equivalent to the standard solution of copper sulfate per milliliter of EDTA

standard solution in ml;

V1 ─ ─ EDTA standard solution volume, ml;

V2 ─ ─ titration of copper sulfate standard solution when the volume of consumption,

ml.

3.5.2 Analysis Procedure :

Titration of iron in the solution after adding 0.015M EDTA standard solution in excess

(for Aluminum, Titanium) 10-15 ml,

then diluted with water to about 200 ml.

Heat the solution to 60 ¯ 70 ℃,

Adjusted to pH 3-3.5 with ammonia (1:1) solution (PH test paper to test precision),

Add 15 ml acetic acid a sodium acetate buffer solution (PH4.2),

boil 12 minutes.

Remove , cool, add 5-6 drops of 0.2% PAN indicator solution to 0.015M standard

solution of copper sulfate titration to bright purple

(The volume of consumption of copper sulfate standard solution denoted V1).

Then add 15 ml of 5% mandelic acid solution,

then heat to boiling for 1 minute.

Remove, cool, Add additional 1 to 2 drops of 0.2% PAN indicator solution, and then

copper sulfate standard solution titration to bright purple

(consumption volume of standard solution of copper sulfate V2).

The percentage of Aluminum oxide content (X4) and the percentage content of

Titanium dioxide (X5) calculated as follows:

TAl2O3 (V-(V1 + V2) K) × 5

X4 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (11)

G × 1000

TTiO2 · V2 · K × 5

X5 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (12)

G × 1000

Where:

TAl2O3 ─ ─ number of milligrams of aluminum oxide equivalent per


TTiO2 ─ ─ ─ number of milligrams of titanium oxide equivalent per


V ─ ─ adding the volume of EDTA standard solution, ml;

V1 ─ ─ when first titration the volume of consumption of copper sulfate standard

solution, ml;

V2 ─ ─ the second titration, the volume of consumption of copper sulfate standard

solution, ml;

K ─ ─ equivalent to the standard solution of copper sulfate per milliliter of EDTA

standard solution in ml;



3.6 Determination of calcium oxide

3.6.1 Reagents

2% potassium fluoride solution:

2 g potassium fluoride (KF · 2H2O) dissolved in 100 ml of water, stored in a

plastic bottle.

Tri yeast amine (1:2):

three ammonium acetate and 1 volume 2 volume of water mixed.

CMP mixed indicator.

20% potassium hydroxide solution.

0.015M EDTA standard solution.


Article 3.2 of the standard draw the prepared sample solution 25 ml, 400 ml beaker

release.

Add 7-8 ml of 2% potassium fluoride solution, and stirring for 2 minutes, then dilute

with water to about 200 ml.

Add 5 ml of triethanolamine (1:2) and small amount of CMP mixed indicator, mixing

add 7 to 8 ml 20% potassium hydroxide solution to a green fluorescence,

(at this time the solution pH> 13),

titration with 0.015M EDTA standard solution to the disappearance of green fluorescence

and red.

Percentage content of calcium oxide (X6) calculated as follows:

TCaO × V1 × 10

X6 = ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (13)

G × 1000

Where:

TCaO ─ ─ number of milligrams of calcium oxide equivalent per

milliliter of standard solution of EDTA ;

V1 ─ ─ titration, the volume of EDTA standard solution consumed, ml;

10 ─ ─ sample solution volume ratio;


3.7 Determination of magnesium oxide

3.7.1 Reagents

10% potassium sodium tartrate solution:

10 g potassium sodium tartrate dissolved in 100 ml of water.

Triethanolamine (1:2)

Ammonia (1:1)

Ammonia - ammonium buffer solution (PH10):

67.5 grams of ammonium chloride dissolved in water, add 570 ml of ammonia,

and then diluted with water to 1 liter (pH meter or precision pH test paper test).

Acid chrome blue K-naphthol green B (1:2.5) mixed indicator:

Weigh 0.30 g acid character blue K and 0.75 g of Naphthol Green B, and 50 g

have been dried at 105 ℃ had mixed small study of potassium nitrate , stored in a jar

mill.

0.015M EDTA standard solution.

Precision pH test paper: PH9.5-13.0.


Article 3.2 of the standard draw the prepared sample solution 25 ml, placed in 400 ml

beaker, diluted with water to about 200 ml.

Add 1 ml of 10% potassium sodium tartrate solution, 5 ml triethanolamine (1:2), then add

20 ml of ammonia - ammonium buffer solution (PH10)

and small amount of acid chrome blue K + naphthol green B (1:2.5) mixed indicator,

titration with 0.015MEDTA standard solution (near the end should go slow drip) pure

blue.

Percentage content of magnesium oxide (X7) calculated as follows:

TMgO (V2-V1) × 10

X7 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (14)

G × 1000

Where:

TMgO ─ ─ number of milligrams of magnesium oxide equivalent per

milliliter of standard solution of EDTA V1 ─ ─ titration of

calcium consumption when the volume of EDTA standard solution, ml;

V2 ─ ─ titration of calcium, magnesium, total consumption volume of EDTA standard

solution, ml;



3.8 Determination of sulfide sulfur

3.8.1 Apparatus and reagents

Magnetic stirrer : 200-300 rev / min.

With ground glass stopper conical flask: volume 250 ml.

Phosphoric acid (1:1):

1 volume of phosphoric acid to the water mixed with equal volume.

0.25% starch solution:

Weigh 0.25 g of starch placed in a small beaker, add a small amount of water, a

paste was injected into 100 ml boiling water, then boil a few minutes, cooling the upper

clear liquid used after the draw (with preparation time).

0.03N potassium iodate standard solution:

Weigh potassium iodate (reference reagent) of about 1.07 g (accurate to 0.0001 g),

placed in a beaker with about 200 ml of cold boiled new dissolved, transferred into 1000

ml volumetric flask in. Then weighed 100 g potassium iodide, 1 g of sodium hydroxide,

in the beaker using the same water-soluble, and then transferred into the volumetric flask

and dilute to the mark with water, shake.

Potassium iodate standard solution of sulfur titer calculated as follows:

G × 0.016 × 1000

Ts = ─ ─ ─ ─ ─ ─ ─ ─ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (15)

35.7

Where:

Ts ─ ─ the number of milligrams of sulfur equivalent per milliliter of standard solution

of potassium iodate;

G ─ ─ the weight of potassium iodate, g;

0.016 ─ ─ equivalent per mg grams of sulfur;

35.7 ─ ─ equivalent grams of potassium iodate.

0.03N sodium thiosulfate standard solution:

Weigh 7.5 g of sodium thiosulfate (Na2S2O3 · 5H2O) placed in a beaker, boiled

cold water with the new solution,

add 0.5 g sodium carbonate, and then transferred into 1000 ml volumetric flask, and in

the same water diluted to the mark, shake, stored in a brown bottle, put it aside for 14

days after the calibration.

Potassium iodate and sodium thiosulfate standard solution volume ratio of the

calibration standard solution:

take the amount of 20 ml burette with potassium iodate standard solution in 250 ml

grinding mouth stuffed with a conical flask,

add 10 ml phosphoric acid (1:1) , stopper, placed in a magnetic stirrer and stir for 1

minute.

Rinse with a small amount of cork and the bottle wall of water, then sodium thiosulfate

standard solution titration added to the yellow solution was about 2 ml 0.25% starch

solution and continue titration with sodium thiosulfate standard solution to the blue

disappears.

Standard solution of potassium iodate and sodium thiosulfate standard solution

volume ratio (K) calculated as follows:

V1

K = ─ ─ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (16)

V2

Where:

K ─ ─ equivalent ml of standard solution of potassium iodate to milliliter of standard

solution of sodium thiosulfate

V1 ─ ─ volume of potassium iodate standard solution, ml;

V2 ─ ─ Jun thiosulfate titration when the consumption volume of standard solution, ml.


Weighed sample of about 0.50 ± 0.02 g (accurate to 0.0001 g), placed in 250 ml

with ground glass stopper of the Erlenmeyer flask, adding accurate under shaking 20 ml

0.03N potassium iodate standard solution,

then add 10 ml of phosphoric acid (1:1), covered with grinding mouth stuffed and placed

on a magnetic stirrer for 1 minute. with a small amount of water washing sidewall to

0.03N sodium thiosulfate standard solution titration, the solution was light yellow . about

2 ml was added 0.25% starch solution and continue with 0.03N sodium thiosulfate

standard solution titration to a blue disappear.

The percentage content of sulfide sulfur (X8) calculated as follows:

Ts (V-V1 · K)

X8 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (17)

G × 1000

Where:

Ts ─ ─ number of milligrams of sulfur. equivalent per milliliter of standard solution of

potassium iodate

V ─ ─ adding potassium iodate standard solution volume, ml;

V1 ─ ─ titration of sodium thiosulfate standard solution when the consumption volume,

ml;

K ─ ─ equivalent ml of standard solution of potassium iodate to milliliter of standard

solution of sodium thiosulfate


3.9 Determination of total sulfur

3.9.1 barium sulfate gravimetric method

3.9.1.1 Reagents

Potassium hydroxide.

Hydrochloric acid (1:1).

0.2% methyl red indicator solution:

0.2 g dissolved in 100 ml of methyl red in ethanol.

Ammonia (1:1).

10% barium chloride solution:

10 g barium chloride dissolved in 100 ml of water.

1% silver nitrate solution:

1 gram of silver nitrate dissolved in 90 ml of water, add 10 ml nitric acid, stored in

a brown bottle.

3.9.1.2 Analysis Procedure

weigh about 0.20 ± 0.01 trial g (accurate to 0.0001 grams), in Nickel crucible.

Add 4 g of potassium hydroxide, cover the crucible lid (leave large gaps), placed on a

small furnace (500-600 ℃) melting 30 minutes.

Remove the crucible and let cool. Leaching with hot water will and melt in 300 ml

beaker, add a few drops of hydrochloric acid (1:1) and hot water ,wash the crucible and

cover.

Add 20 ml hydrochloric acid (1:1),then the solution is heated to boiling, so that melt

completely decomposed. Filter with rapid filter paper, wash with hot water 7-8 times, the

filtrate and the wash collected in 400 ml beaker.

Add 1-2 drops of 0.2% methyl red indicator solution, drop wise ammonia (1:1) to the

solution to turn yellow, then dropping hydrochloric acid (1:1) to the solution until red.

Then add 10 ml hydrochloric acid (1:1), and the solution volume adjusted to 200 ml.

The solution heated to boiling, stirring drop wise 15 ml of 10% barium chloride solution

and continue to boil a few minutes, then moved to warm standing at 2 to 3 hours.

Filter with Quantitative slow filter paper and wash with warm water to the chlorine-

reaction disappeared (test with silver nitrate solution).

Together with the precipitate and filter paper were transferred porcelain crucible and

burn, after ashing furnace at 800 ℃ high temperature burning for 30 minutes. Remove

the crucible, placed in a desiccator to cool to room temperature and weigh. Repeat

burning, until constant weight.

Total sulfur (in sulfur trioxide that) the percentage content (X9) calculated as

follows:

G1 × 0.343

X9 = ─ ─ ─ ─ ─ ─ × 100 - - - - - - - - - - - - - - - - (18)

G

Where:

G1 ─ ─ the weight of precipitate after ignition, g;

0.343 ─ ─ barium sulfate sulfur in the three amide conversion factor;


3.9.2 Combustion - and in Furance

3.9.2.1 Instrument devices and reagents

Burner:

silicon carbide or silicon carbide tube heating, temperature can be maintained at

1300 ℃, constant temperature with 80 ¯ 100 mm.

Combustion tube:

750 mm long corundum tube reducers. One end of the outer diameter 22 mm,

diameter 19 mm, length 690 mm; other end of the outer diameter of 10 mm, diameter 7

mm, length 60 mm.

Temperature control:

Control the temperature range 0 ¯ 1600 ℃.

Platinum and a platinum-rhodium thermocouple.

Burning Boat:

Corundum boat or refractoriness greater than 1400 ℃ in porcelain boat, length 75-

90 mm, the width of 12-14 mm, 8-10 mm high. Advance in the use of dilute hydrochloric

acid (1:6) in boiling, wash with water after drying on a small stove, save in the backup

device is dry.

Nickel-chromium wire push rod:

diameter of about 2 mm, length 650 mm, one end of the roll into about 10 mm

diameter circular spiral pad, as used to promote the burning boat (push the stick to make

two marks: First, push the burning boat to the furnace temperature to 700 ℃ at a distance,

one push from the center of high temperate).

Nickel-chromium wire hooks:

diameter of about 2 mm, length 650 mm, one end bent into a small hook, as the pull

boat with burning.

T-shaped glass tube:

Install push rod with a double into the air.

Glass tee Pistons:

7 to 8 mm outer diameter, inner diameter of 5 to 6 mm, washing.

Three-way piston burettes:

capacity of 25 ml.

Gas flowmeter:

the maximum range of 1000 ml / min.

Vacuum pump:

2X-1A-type rotary vane vacuum pump or similar properties, extraction rate of 1 l /

sec.

Wash bottle:

capacity of 250 ml, 2, respectively, loaded 130 ml of 15% copper sulfate solution and

100 ml of sulfuric acid, air purification purposes.

Sulfur absorber set:

capacity of 250 ml, 2 with the sintered glass sand as dispersing gas, the gas filter,

glass melting plate for the G1 type.

Drying tower:

capacity of 250 ml, of which 2 / 3 volume of sodium loading lime, 1 / 3 volume

loaded silica gel.

Silicone rubber tube:

outside diameter 11 mm, internal diameter 6 mm, and fixed combustion tube

connecting the absorption of sulfur Used.

Mixed flux:

to 10 g of quartz powder, 10 grams of ferric oxide and 20 g of graphite powder in an

agate mortar in the milk and mix small study, stored in the mill jar.

Bromocresol green-methyl red mixed indicator solution:

0.3 g and 0.2 g of bromocresol green-methyl red dissolved in 100 ml of ethanol,

shake.

0.3% hydrogen peroxide solution:

10 ml 30% hydrogen peroxide mixed with 880 ml of water, shake, stored in a plastic

bottle.

0.025N sodium hydroxide standard solution,

to 10 g sodium hydroxide dissolved in 10 liters of water, shake well, stored in a belt

stopper (with the lime drying tube) of the cover glass bottles or hard plastic bottles.

Calibration method:

Weigh about 0.1 g of potassium hydrogen phthalate (accurate to 0.0001 g), placed in

300 ml beaker, add 150 ml of cold boiled new (the cold water and with sodium hydroxide

solution to phenolphthalein reddish ) to dissolve.

Then add 5 ¯ 6 drops of 1% solution of phenolphthalein indicator, titration with sodium

hydroxide standard solution to reddish.

Sodium hydroxide standard solution of sulfur trioxide titer calculated as follows:

G × 0.04003 × 1000

Tso3 = ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ × 1.016 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (19)

V × 0.2042

Where:

Tso3 ─ ─ the number of milligrams of sulfur trioxide. is equivalent to milliliter of

standard solution of sodium hydroxide

G ─ ─ the weight of potassium hydrogen phthalate, grams.


0.04003 ─ ─ equivalent per mg of the number of grams of sulfur trioxide,

0.2042 ─ ─ equivalent per mg of potassium hydrogen phthalate grams;

1.016 ─ ─ correction factor.

3.9.2.2 Analysis Procedure

Schematic diagram of the apparatus installed by post (from the stove burner mouth until

the end of the previous absorber to keep the total length of 150 mm or so), transmission

temperature to 1300 ℃. Sulfur absorber in each set into the 120 ¯ 130 items 毫升 0.3%

hydrogen peroxide solution and 10 drops of bromocresol green - methyl red mixed

indicator solution, start pump, adjust the air flow of 600 ml / min or so, and to 0.025N

standard solution of platinum hydroxide solution to adjust the absorption of light green.

Weighed sample of about 0.1 grams (accurate to 0.0001 g), placed in a pre-mix has been

paved with 0.2 g flux inside the burning boat, with a fine glass rod and mix well. Remove

the combustion tube with the inlet side of the bat and then there are T-shaped glass tube

of the rubber stopper, the burning boat to release the nozzle, and then plugged the rubber

stopper. Nickel-chromium wire and then push the stick to push the burning boat to the

location of the furnace temperature at 700 ℃, start the vacuum pump, to maintain air

flow at 600 ml / min about 1 minute before the pre-burn combustion boat with a push

stick to push the center of high temperate position, and immediately withdrew the

vertebral rod, so as to avoid distortion. Wait 10 minutes after combustion, titration with

0.025N sodium hydroxide standard solution, to absorb the liquid from red to green. Then

add water to wash tee piston 4 to 5 times (each about 2 ml of water) to wash away the

acid left in the pipe, this time to absorb fluid and from green to red and continue titration

with standard sodium hydroxide solution to the light the green. The second absorber to

absorb liquid, if the color changes, likewise on the titration to bright green. Close the

vacuum pump, open the inlet side of the combustion tube rubber stopper, nickel-

chromium wire with a hook out of the combustion boat, and then another by the operation

of the continuous measurement for continuous sample measurement, the standard

solution used in 0.025N sodium hydroxide consumption of more than 25 ml, the required

replacement of the absorption liquid.

Total sulfur (in sulfur trioxide that) the percentage content (X9) calculated as

follows:

Tso3 · V

X9 = ─ ─ ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (20)

G × 1000

Where:

Tso3 ─ ─ the number of milligrams of sulfur trioxide. is equivalent to milliliter of

standard solution of sodium hydroxide

V ─ ─ titration consumes standard solution of sodium hydrogen prostrate volume, ml;


3.10 Determination of sulfate sulfur

Sulfate sulfur (as sulfur trioxide)

the percentage content (X10) calculated as follows:

X10 = X9-X8 × 2.5 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (21)

Where:

X9 ─ ─ according to section 2.9 of this standard measured by the percentage of total

sulfur content;

X8 ─ ─ according to Rule 3.8 of the standard voltage was the percentage content of

sulfide sulfur;

2.5 ─ ─ factor of. sulfide sulfur trioxide conversion

3.11, potassium hydroxide, sodium oxide determination

3.11.1 Instruments and reagents

highly performance flame photometer.

Sulfuric acid (1:1):

the same volume of sulfuric acid slowly into the water.

Hydrofluoric acid.

0.2% methyl red indicator solution.

Ammonia (1:1).

Hydrochloric acid (1:1).

10% ammonium carbonate solution:

10 g ammonium carbonate dissolved in 100 ml of water (used when the

preparation).

Potassium hydroxide, sodium oxide standard solution:

Weigh accurately bake in 130-150 ℃ over 2 hours of potassium chloride and

sodium chloride 0.943 g 0.792 g, placed in a beaker of water dissolved, transferred into

1000 ml volumetric flask, diluted to the mark with water, shake. This standard solution of

potassium hydroxide equivalent per ml and 0.50 mg of sodium oxide.

3.11.2 Potassium hydroxide, sodium oxide working curve drawing

Burette to 7 with 100 ml volumetric flask, respectively, into the 1.00, 2.00, 4.00,

6.00,8.00, l0.00, 12.00 potassium hydroxide, sodium oxide standard solution (potassium

and sodium oxide equivalent, respectively, of 0.50, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00 mg),

diluted to the mark, shake. Then click on each instrument in the flame photometer were

measured using the procedures, according to the measured galvanometer reading and the

relationship between the concentration of the solution, potassium hydroxide and sodium

oxide, respectively, draw the working curve.


Weigh 0.1-0.2 grams of sample (accurate to 0.0001 g), placed in platinum (or gold) dish

with a small amount of water wetting. Add 15-20 drops of sulfuric acid (1:1) and 5-10 ml

of hydrofluoric acid, placed in low-temperature hot plate evaporation, nearly dry shake

platinum dish to splash loss. After the drive to do to be hydrofluoric acid, gradually

increasing the temperature, sulfur trioxide white smoke continued to drive to do. Remove

and let cool. Add about 50 ml of hot water, and crushed to dissolve the residue. Add 1

drop of 0.2% methyl red indicator solution with ammonia (1:1) and to yellow, then add

10 ml of 10% carbonate solution, stirred, placed in the electric panel heating for 20-30

minutes. With rapid filter paper, wash with hot water, filtrate and lotion containing a 100

ml volumetric flask. After cooling to room temperature, with hydrochloric acid (1:1) and

to the solution was slightly red, and then diluted to the mark with water, shake to the

flame photometer were measured by instrumentation procedures.

Potassium hydroxide, sodium oxide percentage content (X11, X12) calculated as

follows:

C1

X11 = ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (22)

G × 1000

C2

X12 = ─ ─ ─ ─ ─ ─ × 100 ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ ⋯ (23)

G × 1000

Where:

C1 ─ ─ the working curve was determined per 100 ml solution of potassium content, mg;

C2 ─ ─ the working curve was measured in 100 ml of sodium oxide content of the

solution, mg;


Appendix A permissible error of measurement results (Supplement)

A.1 Determination of the allowable error range results as follows:%

━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ┯ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ┯ ━ ━ ━ ━ ━

━ ━ ━ ━ ━ ━ ━ ━

Determination of the project │ │ indoor permissible error tolerance between room

─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ┼ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─ ┼ ─ ─ ─ ─ ─ ─ ─ ─ ─ ─

Loss on ignition │ 0.15 │ ━

SiO2 │ 0.25 │ 0.40

Fe2O3 │ 0.15 │ 0.25

Al2O3 │ 0.25 │ 0.40

TiO2 │ 0.15 │ 0.20

CaO │ 0.25 │ 0.40

MgO │ 0.20 │ 0.30

Total sulfur (in SO3 said) │ 0.25 │ 0.40

Sulfate sulfur (as SO3 said) │ 0.25 │ 0.40

S │ 0.10 │ 0.15

K2O │ 0.10 │ 0.15

Na2O │ 0.10 │ 0.15

━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ┷ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ━ ┷ ━ ━ ━ ━ ━

━ ━ ━ ━ ━ ━ ━ ━

A.2 Some notes on tolerance

A.2.1 This standard permit listed in error, are the absolute error.

A.2.2 In the same test room, using the standard method when analyzing the same sample,

each item to be independently measured twice, the average value as reported values. If

the results exceed the two indoor allowable error range, a third should be measured, the

results obtained with any of the previous two or the difference between the results of an

analysis of the indoor meet tolerance requirements, then the average value as the reported

values. Otherwise, you should find out the reasons, re-analyzed according to the above

provisions.

A.2.3 two laboratories, using the standard methods to analyze the same sample each time,

the results of each project should be consistent with the average difference between the

allowable error room requirements. Dispute, another unit should be agreed to arbitration

in accordance with this standard analysis. Reported in the results of the arbitration unit

subject, compared with the original analysis, if the difference between two results in line

with the provisions of room between the permissible error is that the original analysis is

correct, if tolerance is not considered accurate.

Additional Comments:

The standard proposed by the Building Materials Research Institute, under the

jurisdiction of the Building Materials Research Institute.

The standard by the Institute of Building Materials Research Institute is responsible for

the drafting of the cement.

The main drafters servant, Hu Yong, E King piano.

The standard commission Cement Research Institute of Building Materials Research

Institute responsible for the interpretation.

complete chemical analysis of portland cement

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