طريقة الفحص الكيميائي لمادة الاسمنت

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السلام عليكم .... كيف حالكم يا كيميائيين
ارجوا منكم مساعدتي في الحصول على طريقة الفحص الكيميائي لمادة الاسمنت ، أو اي شيء يوصلني الى حساب نسب المواد المتكون منها الاسمنت ، .... وجزاكم الله خيراً :20:
 

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العملية تستوجب اجراء تحليل كيميائي مختبري او جهاز ( x - ray analysiser) لمعرفة مكونات الاسمنت واذا يوجد لديك مثل هذه الامكانية ممكن احملك طريقة العمل المختبرية الكيميائية مع خالص تحياتي
 

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procedure to chemical analysis

METHODS OF TEST FOR THE CHEMICAL
ANALYSIS OF PORTLAND CEMENT,
FLY ASH, POZZOLAN, AND BLENDED CEMENT
CAUTION:Prior to handling test materials, performing equipment setups, and/ or conducting this
method, testers are required to read “SAFETY AND HEALTH” in Part 3 of this method. It is the responsibility of the user of this method to consult and use departmental safety and health practices and determine the applicability of regulatory limitations before any testing is performed.
SCOPE
This test method is divided into the
following parts:
1. Determination of Major Constituents of
Portland Cement
2. Determination of Chlorides
3. Safety and Health
PART 1. DETERMINATION OF MAJOR
CONSTITUENTS OF
PORTLAND CEMENT
The procedures used in the chemical analysis of portland cement are described in this group of tests. For routine samples, the atomic absorption method is used.
For referee samples, or samples where there is a question as to the results, the official methods described in ASTM Designation: C 114 are used.
A. APPARATUS
1. Unless otherwise indicated, all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society (where such specifications are available).
2. Atomic Absorption Spectrophotometer - (AAS) - The Perkin-Elmer AAnalyst 100 has been found to be satisfactory.
3. Carbon and Sulfur Analyzer - The LECO Corp. Model CS-225 induction furnace has been found satisfactory.
B. PROCEDURE
Before testing, pass samples through a 850-µm sieve in order to mix the sample, break up lumps and remove foreign materials. Discard foreign materials and hardened lumps that do not break up on sieving or brushing.
Store the cement in airtight moisture proof containers to prevent aeration or absorption of moisture prior to test.
1. Rapid Chemical Analysis Method:
The determination of oxides of silica, aluminum, iron, calcium, magnesium, sodium and potassium using an atomic absorption spectrophotometer and that of sulfur trioxide using the LECO induction furnace are described in the method.
California Test 404
August, 1998
- 2-
a. Selection of National Institute of Standards and Technology (NIST) Standards:
Select a series of at least four standard cement samples that will bracket the expected concentrations of the elements in the unknown samples.
b. Preparation of Standards:
Weigh 0.250 g of NIST standard
cement into a
100-mL beaker. Disperse with 20 mL of distilled water and 4 mL of concentrated hydrochloric acid. Break up lumps of cement with a rubber policeman or glass stirring rod, rinse and remove the policeman or rod from the beaker. Cover the sample with a watch glass and digest the sample on a low hot plate for 15 min at approximately 75˚C. During digestion, continuously stir the sample. An oscillating hot plate is preferred for this process. Filter through a medium-texture filter paper into a 200-mL volumetric flask, scrubbing the beaker with a rubber policeman. Wash the sample thoroughly with hot hydrochloric acid (1:99), then with several rinses of hot distilled water.
Cool the sample to room temperature, then dilute to a volume of 200 mL. It is recommended that new standards be made up each month.
c. Preparation of Samples:
Weigh 0.125 g of cement into a 100-mL beaker. Disperse it with 10 mL of d istilled
water
and
2 mL of
concentrated
hydrochloric
acid . Digest and prepare the sample exactly as described in Section b, “Preparation of Standards.” The final filtrate is diluted to a volume of 100 m L.
For the determinations of calcium oxide and magnesium oxide, a portion of the solutions prepared in Sections b
and c are diluted to 1 to 10 with the final dilution containing 0.5 % of lanthanum, which is found to be effective for the suppression of chemical interferences.
Standards
are diluted similarly.
d. Preparation of Fly Ash, Pozzolan,
and Blended Cement Samples:
Follow the procedures as described in ASTM Designations: C 311 and C 595, except modify the fusion procedure as follows. A quantity of the ignited sample, equivalent to 0.250 g of the moisture free sample, is mixed with 1.5 g of an equal mixture of Li2B4O7
and LiBO2. The fusion procedure
is described in ASTM Designation: E 886. The fused mixture is then dissolved in 80 mL of 1:8 hot hydrochloric acid.
The resulting solution is filtered and finally diluted to 200 mL. NIST standards for calibration are prepared in the same way.
e. Sulfur Trioxide Determination Using
an Induction Furnace:
Follow the manufacturer's recom- mendations. The following has been found to be a satisfactory method using a LECO induction furnace.
Weigh a 0.15 g sample into a combustion crucible. Add one scoop of Lecocel and one scoop of iron chip accelerator. Follow the instrument manufacturer’s directions for this analysis. Standardize the instrument with NIST cement standards using the same procedure as described above.
2. Reference Analysis
For silica, ammonium hydroxide group, aluminum oxide, ferric oxide, calcium oxide, magnesium oxide, sulfur trioxide, ignition loss, insoluble residue, sodium oxide and potassium oxide, follow ASTM Designation: C 114.
California Test 404
August, 1998
- 3-
PART 2. DETERMINATION OF CHLORIDES
This part describes a procedure for deter- mining chlorides in portland cement and portland cement concrete.
A. APPARATUS
1. Chloride specific ion electrode
2. Double junction reference electrode
3. Millivoltmeter compatible with the
electrodes
B. PROCEDURE
1. Weigh 2.0 to 5.0 g of portland cement into
a 400-mL breaker.
2. Add 100 mL of boiling water.
3. Add a slight excess of 0.1 Normal silver nitrate from a buret (5 mL is an approximate amount of silver nitrate for cement that contains no more than 0.15 % chloride). Record the amount added.
4. Boil the sample for two minutes, remove
it from the heat, then cool it slightly.
5. Slowly add 20 mL of concentrated nitric
acid, efflorescence will often occur.
6. Heat and break up any lumps of undissolved cement with the flattened end of a stirring rod, cover the sample and boil it for 2 min.
7. Filter through a medium speed (90-mm “OK” is satisfactory) paper in a Buchner funnel with suction. The filtrate should be clear.
Add approximately 1 g of diatomaceous earth to aid filtering if desired.
8. Wash the residue three times with 1:99
nitric acid. Discard the residue.
9. Quantitatively transfer the filtrate to a 400-mL beaker and cool it to room temperature.
10. Carry three standards through the test procedures with the same amount of acid and silver nitrate but without cement.
11. Adjust all standards and samples to
approximately
equal volume
with
distilled water to eliminate blank
determination.
12. Titration of Samples:
a. Titration using a ferric ion indicator. With cements that are low in iron, add a few drops of ferric iron indicator (5 g of ferric ammon- ium sulfate dissolved in 50 mL of 1 Normal nitric acid). Titrate with
0.05
Normal
ammonium thiocyanate that has been stand- ardized against the silver nitrate standards to the first permanent red color.
Use burets with 0.05-mL graduations and make all readings carefully to the nearest 0.01 mL.
b. Titration
with
a
specific ion
electrode.
Following the
manu-
facturer's recommendation for the use of specific ion electrode, titrate the samples with the 0.05 Normal ammonium thiocyanate that has been standardized against the silver nitrate standards prepared in Step 10. Plot a curve of the change in potential
against
volume
of
thiocyanate to find the end point.
13. Calculate chlorides by the following
formula:
% chlorid es = [(A x N ) - (B x M)] x F x
100/ mass
of the sample, to the
nearest 1g
Chlorine (ppm) = % x 10 000
Where A = mL of AgNO3
N = Normality of the AgNO3
 

توفي2006

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abue tycer اخي الحبيب جزاك الله خير الجزاء وجعله الله في ميزان اعمالك
انا اريد اجراء تحليل كيميائي مختبري لاني لا املك جهاز x - ray analysiser
ارجوا منك اخي العزيز التوضيح لي ماهي الادوات المطلوبة و ماهي المواد الكيميائية المستخدمة في هذه الفحوصات .
وانواع الفحوصات المطلوبة للكشف عنها في مادة الاسمنت هي كالاتي :
محتوى المواد الغير قابلة للذوبان
محتوى ثاني اوكسيد السيليكون
محتوى الالمنيوم
محتوى اوكسيد الحديديك
محتوى اوكسيد الكالسيوم
الومنيات ثلاثي الكالسيوم
محتوى ثالث اوكسيد الكبريت
الفقدان بالاحتراق
عامل الاشباع الجيري


لطفاً وليس امراً ارجوا ان تكون الطريقة باللغة العربية قدر الامكان واذا لم تتوفر بالعربية لا مانع منها ان تكون باللغة الانكليزية .... وجزاك الله خيراً وقدرك على فعل الخير
 

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حداول مكونات المواد الاولية لاسمنت

Raw material of cement factory in Iraq


clay
limeston
Sample component
19.9
40.85
Loss on ignition
40.18
6.19
SiO2
8.4
0.9
Al2O3
4.34
0.33
Fe2O3
0.62
0.06
TiO2
18.74
48.83
Cao
5.29
2.64
MgO
0.14
0.41
SO3
0.75
0.03
K2O
0.03
0.03
Cl
0.16
0.03
P2O5
3.15
1.95
- -
- -
SILICA RATIO
ALUMINA RATIO
 

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مكونات الكلنكر

Theoretical raw mixture calculation & clinker



Clinker



Raw meal



Components



76.2



% limestone



22.2



% clay



1.6



% Fe – carrier



35.46



% loss on ignition



21.18



13.67



% SiO2



4.06



2.62



% Al2O3



4.08



2.64



% Fe2O3



0.28



0.18



% Ti O2



64.09



41.37



%CaO



4.93



3.19



% MgO



0.52



0.34



% SO3



0.64



0.41



% K2O



0.29



0.19



% Na2O



0.03



% Cl



96.0



Lime standard



2.6



Silica ratio



5.2



Silica acid ratio



1.0



Alumina ratio



66.8



% C3S



10.4



%C2S



3.9



% C3A



12.4



C4AF
 

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شهادة فحص الاسمنت العادي

شهادة فحص واختبار السمنت العادي لمعامل السمنت في احد معامل الاسمنتOrdinary Portland cement Test certificat

PHYISICAL TESTS
CHEMICAL ANALYSIS
Compressive strength kg per sq cm
Tensile strength
Silica ----- sio2 -----21.73 %
Insoluble Residue ---0.2 %
Alumina ---- Al2o3 ---- 5.45%
Ferric oxide ----- Fe2o3 ---- 3.11 %
Lime ------Cao ----- 63.40 %
Magnesia ------ Mgo ---- 2.6 %
Sulphuric Anhydried ---SO3 ---- 2.49 %
Losse on Ignition ------ 1.18 %
Total alkalies as ----- Na2o ---- 0.70
Free lime ---------- % , C4AF 9.4%
C3S 45.3 % , LSF 0.89 , C2S 28 % ,
C3A 9.2 %
28 days
7 days
3 days
28 days
7 days
3 days
-------
400
331.97
-----
-----
-----
Fineness
Residue on B . S . mesh no 170
3.6 %
SETTING TIME
Intial ------- 150 mins
Final ------- 3 hrs
SPECIFIC SURFACE
Blaine --------2973 ---- sq cm per gm
Percentage water
To give apaste of standard
Consistency : 27 %
Compressive strength : 10 %
Setting time : 27 %
Soundness ( Lachatelier )
Expansion without aeration ---- 1.0 mm.
The above Tests have been carried out in accordance with the requirements of B . S .
 

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شهادة فحص وأختبار السمنت المقاوم للأملاح لمعاملSulphate Resisting cement test certificat

Physical tests

Chemical analysis

Specific surface
Compressive strength kg sq cm


Silica------ Sio2 – 28.24 %
Insoluble residue ----- 0.41 %
Alumna ------ Al2o3 – 3.58 %
Ferric oxide ------FE2O3 – 5.32 %
Lime -------- Cao – 63.84 %
Magnesia --------- Mgo – 1.84 %
Sulphuric anhydride----- So3 – 1.61 %
Loss on ignition ----------------0.85 %
Total alkalies 99.33
Na2o = 0.75 %
Free lime ----------- %, C4AF 16.3 % , C3S 54.5 %,
LSF 0.90 , C2S 22.5 %, C3A 0.4 %
C4AF + 2C3A ------------------- 17.1 %

Blaine ) sq cm per gm )
3298
22 days
7 days
3 days


211
105
------

Required

Residue on mesh 170
1.8 %
Residue on
Mesh 72
0.2 %
327
220
135

Test results


Tensile strength kg per sq cm ASTM C -150
Time of setting
A S T M
C - 150
Time of setting
B . S
4027
22 days
7 days
3 days



22.8
17.6
--------------

Required

Intial : 140 mins
Final : 3:15 hrs
40.8
22.5
17.8

Test results


Compressive strength kg per sq cm B. S 4027
AUTOCLAVE
LECHATELIER
28 days
7 days
3 days


The above test have been carried out in accordance with the requirements of both B . S . 4027 , ASTM C – 150 & I . S . O NO 6 : 68 of Sulphat Resisting cement

----------
239
155

Required
0.005 %
1 mm
----------
341
227

Test results

 

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جزيت خيراً اخي ابو تيسير وبارك الله فيك
 

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النــوع : سمنتعادي (طاسلوجة )
أولأ :الفحوصات الكيميائية .
The limit of specification according to Iraq Specification No.5/1984
Result (%)
Type of test
-
19.4
Sio2
-
4.41
AL2O3
-
2.76
Fe2O3
-
63.45
CaO
Not more than 5%
2.5
MgO
Not more than 2.5%
2.12
SO3
Not more than 4%
3.21
L.O.I
Not more than 1.5 %
0.80
I.R
0.66 - 1.02
0.80
L.S.R
-
0.55
C3A
* The sample (satisfied) the chemical Requirements of Iraq specification
No.5/1984


الفحوصاتالفيزيائية :-



The limit of specification according to Iraqi specification No.5/1984​
Result​
Type of test​
Not less than 45 min.​
145 min​
Initial​
Setting time(min)​
Not More than 10 hr
3.50 hr​
Final​
Not more than 0.8
0.7​
Soundness (%)​
Expansion Lechatleier​
Not less than (15) Mpa​
23.7 Mpa​
For (3)day​
Compressive Strength (Mpa)​
Not less than(23) Mpa​
25.7 Mpa​
For (7)day​
Not less than 2300​
(cm[SUP]2[/SUP]/gm)​
2420​
Fineness (cm[SUP]2[/SUP]/gm) by Blaine Method​
* The sample(satisfied) the Physical Requirements of Iraq Specification​
No.5/1984 .​












مهندس استشاري :لؤي خليل سلمان

 

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ممكن طريقة الفحص بالاشعة السينية
 
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