CN109596547A - The spectroscopic methodology of oxide content in a kind of rapid and accurate determination cement - Google Patents
The spectroscopic methodology of oxide content in a kind of rapid and accurate determination cement Download PDFInfo
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Abstract
The present invention discloses a kind of spectroscopic methodology of oxide content in rapid and accurate determination cement, belongs to the detection technique field of cement.The principle of the present invention is that the intensity of spectral line of test substance is directly proportional with its solution concentration in the curve obtained using inductively coupled plasma emission spectrography: weighing the standard sample and sample to be tested of phase homogenous quantities, under extension rate unanimous circumstances, the intensity of spectral line of test substance is directly proportional with its content, according to its intensity, its content can be acquired on standard curve.Specific operating procedure includes claiming sample, sintering, dissolution, constant volume, drawing standard curve, measure the content of oxide in cement sample to be tested, average.The present invention can rapidly and accurately measure SiO in cement by once test using inductively coupled plasma emission spectrography simultaneously2、Al2O3、Fe2O3And CaO content, have the advantages that accurate, efficient, economical, environmentally friendly, easy to operate.
Description
Technical field
The invention belongs to the detection technique fields of cement, are more specifically related to oxide in a kind of rapid and accurate determination cement
The spectroscopic methodology of content, mainly using inductively coupled plasma atomic emission come SiO in rapid and accurate determination cement2、Al2O3、
Fe2O3, CaO content.
Background technique
Cement is a kind of powdery hydraulicity inorganic coagulation material, forms slurry after adding water and stirring, can harden in air or
Person is preferably hardened in water, and can the materials such as sand, stone are cemented together securely.Coagulation is made using cementing rubble
Soil, not only intensity is higher after curing, and can also resist the erosion of fresh water or brackish water.Therefore, cement is used as always one kind
Important cementitious material is widely used in the engineerings such as civil construction, water conservancy, national defence.
The main chemical compositions of cement have silica SiO2, aluminum oxide Al2O3, di-iron trioxide Fe2O3And oxidation
Calcium CaO.Currently, analysis cement main chemical compositions are mainly to be tested according to GB/T 176, but such test method exists
Following shortcomings: such as low efficiency, learning cost are high, operation difficulty is big, more than required reagent type etc..For example, one
A testing crew tests SiO in cement using conventional method2、Al2O3、Fe2O3, tetra- kinds of oxides of CaO content, tested
As a result 3 day time is taken around, testing efficiency is extremely low.
Summary of the invention
The purpose of the present invention be exactly the shortcoming being directed in the presence of the above-mentioned prior art and provide it is a kind of quick and precisely
Measure the spectroscopic methodology of oxide content in cement.The present invention is using inductively coupled plasma emission spectrography by once testing
SiO in cement can be rapidly and accurately measured simultaneously2、Al2O3、Fe2O3And CaO content, there is accurate, efficient, economy, ring
It protects, advantage easy to operate.
The purpose of the present invention can be realized by following technique measures:
The spectroscopic methodology of oxide content includes the following steps: in rapid and accurate determination cement of the invention
A, claim sample: weighing the cement standard sample of three parts of different labels and the cement sample to be tested of two parts of identical labels respectively, often
Part quality is 0.1000g, and is sequentially placed in five identical silver crucibles；
B, it is sintered: being separately added into the granular sodium hydroxide of 2.0g in five silver crucibles into step A, and be uniformly mixed；So
Five silver crucibles are put into 700 DEG C of Muffle furnace afterwards and are heated, are melted 15~20 minutes；
C, it dissolves: the 1+1 hydrochloric acid solution of 20 mL being added into five 250 mL volumetric flasks；One is inserted into each volumetric flask
A long neck funnel；Five silver crucibles are successively taken out, the end suitable for reading of corresponding long neck funnel is put into after natural cooling；By boiling water plus
Enter into each crucible, after fusant falls off, washs crucible with boiling water, crucible and earthenware are then washed with 1+1 hydrochloric acid solution
Crucible lid is collected cleaning solution together into each corresponding volumetric flask；
D, constant volume: five volumetric flasks are placed in cold bath and are cooled to room temperature；Then it plus water, shakes up, and is settled to scale, obtain
Three parts of cement standard sample solutions and two parts of cement testing sample solutions；
E, it draws standard curve: the obtained three parts of cement standard sample solutions of step D is successively introduced into inductively coupled plasma
In body emission spectrometer, the instrument parameter of optimization is set, with SiO in cement standard sample solution2、Al2O3、Fe2O3, CaO contains
Amount is abscissa, draws standard curve by ordinate of the intensity of emission spectra of Si, Al, Fe, Ca；
F, it measures the content of oxide in cement sample to be tested: a cement testing sample solution in step D is introduced into inductance
In coupled plasma optical emission spectrometer, identical with step E instrument parameter is set, Si in measurement cement testing sample solution,
The spectral intensity of Al, Fe, Ca, and cement is checked according to the corresponding relationship of spectral intensity and content in the standard curve of step E
SiO in testing sample solution2、Al2O3、Fe2O3, CaO content；Then, repetitive operation waits for another cement in step D
Sample solution be measured in parallel；
G, it averages: according to being measured twice in step F as a result, acquiring SiO in cement testing sample solution respectively2、Al2O3、
Fe2O3, CaO respectively correspond to the average value of content.
Heretofore described sodium hydroxide is that analysis is pure, and hydrochloric acid solution is excellent pure grade, and water is level-one water.
The model Agilent Technologies of heretofore described inductive coupling plasma emission spectrograph
5110 ICP-OES；Set optimization instrument parameter: read access time be 5 s, RF power be 1200W, stablize the time be 10 s,
View mode is radial direction, height of observation is 8 mm, atomization gas flow is 0.70 L/min, plasma flow amount is 12.0 L/
Min, secondary air amount are 1.00 L/min.
The characteristic spectral line of heretofore described Si, Al, Fe, Ca are successively selected as Si:288.158 nm, Al:396.152
Nm, Fe:238.204 nm, Ca:317.933 nm.
Design principle of the invention is as follows:
The present invention be in the curve obtained using inductively coupled plasma emission spectrography the intensity of spectral line of test substance and its
Solution concentration is directly proportional: the standard sample and sample to be tested of phase homogenous quantities are weighed, it is to be measured under extension rate unanimous circumstances
The intensity of spectral line of substance is directly proportional with its content, and according to its intensity, its content can be acquired on standard curve.
Advantageous effects of the invention are as follows:
The present invention can be measured rapidly and accurately using inductively coupled plasma emission spectrography by once test simultaneously
SiO in cement2、Al2O3、Fe2O3With CaO content (primary experiment only about need 4 hours), have it is accurate, efficiently, economic, environmental protection,
Advantage easy to operate.
Specific embodiment
The present invention is further described below with reference to embodiment:
It is now that technical parameter Unify legislation involved in the specific embodiment of the invention is as follows to avoid repeated description:
Heretofore described sodium hydroxide is that analysis is pure, and hydrochloric acid solution is excellent pure grade, and water is level-one water.
The model Agilent Technologies of heretofore described inductive coupling plasma emission spectrograph
5110 ICP-OES；Set optimization instrument parameter: read access time be 5 s, RF power be 1200W, stablize the time be 10 s,
View mode is radial direction, height of observation is 8 mm, atomization gas flow is 0.70 L/min, plasma flow amount is 12.0 L/
Min, secondary air amount are 1.00 L/min.
The characteristic spectral line of heretofore described Si, Al, Fe, Ca are successively selected as Si:288.158 nm, Al:396.152
Nm, Fe:238.204 nm, Ca:317.933 nm.
Embodiment one
Embodiment one includes the following steps:
A, claim sample: the cement standard sample weighed respectively marked as GSB08-1533-2003, GSB08-1537, GBW03206 is each
Portion, weigh two parts marked as GBW03201b identical cement samples to be tested (cement sample marked as GBW03201b for
Buying for user is sample to be tested, needs to obtain SiO in cement by spectroscopic methodology of the invention2、Al2O3、Fe2O3With
The measured value of CaO content, referring to table 3；Cement sample marked as GBW03201b is standard sample for production and sales side
Product have been labeled with SiO in cement when dispatching from the factory sale2、Al2O3、Fe2O3With the standard value of CaO content, referring to table 1), every part
Quality is 0.1000g, and is sequentially placed in five identical silver crucibles.
B, it is sintered: being separately added into the granular sodium hydroxide of 2.0g in five silver crucibles into step A, and mix equal
It is even；Then five silver crucibles are put into 700 DEG C of Muffle furnace and are heated, melted 15~20 minutes.
C, it dissolves: the 1+1 hydrochloric acid solution of 20 mL being added into five 250 mL volumetric flasks；It is inserted into each volumetric flask
Enter a long neck funnel；Five silver crucibles are successively taken out, the end suitable for reading of corresponding long neck funnel is put into after natural cooling；It will boiling
Water is added in each crucible, after fusant falls off, is washed crucible with boiling water, is then washed crucible with 1+1 hydrochloric acid solution
And crucible cover, cleaning solution is collected together into each corresponding volumetric flask.
D, constant volume: five volumetric flasks are placed in cold bath and are cooled to room temperature；Then it plus water, shakes up, and is settled to scale,
Respectively obtain a GSB08-1533-2003 cement standard sample solution, portion GSB08-1537 cement standard sample solution, one
Part GBW03206 cement standard sample solution and two parts of GBW03201b cement testing sample solutions.
E, it draws standard curve: the obtained three parts of cement standard sample solutions of step D is successively introduced into inductive coupling etc.
In ionomer emission spectrum instrument, the instrument parameter of optimization is set, with SiO in cement standard sample solution2、Al2O3、Fe2O3、CaO
Content be abscissa, draw standard curve by ordinate of the intensity of emission spectra of Si, Al, Fe, Ca.
F, the content of oxide in cement sample to be tested is measured: by a GBW03201b cement sample to be tested in step D
Solution is introduced into inductive coupling plasma emission spectrograph, sets instrument parameter identical with step E, measures GBW03201b
The spectral intensity of Si, Al, Fe, Ca in cement testing sample solution, and according to spectral intensity and content in the standard curve of step E
Corresponding relationship check in SiO in GBW03201b cement testing sample solution2、Al2O3、Fe2O3, CaO content (referring to table 2)；
Then, repetitive operation be measured in parallel to another GBW03201b cement testing sample solution in step D.
G, it averages: according to being measured twice in step F as a result, to acquire GBW03201b cement sample to be tested respectively molten
SiO in liquid2、Al2O3、Fe2O3, CaO respectively correspond to the average value of content, referring to table 3.
Each content of material statistical form in the standard sample of 1 embodiment one of table
The parametric statistics table of each element in the standard curve of 2 embodiment one of table
| Element | Spectral line/nm | Linearly dependent coefficient |
| Si | 288.158 | 0.9999 |
| Al | 396.152 | 0.9999 |
| Fe | 238.204 | 0.9994 |
| Ca | 317.933 | 0.9997 |
The standard value of each content of material and the contrast table of measured value in 3 sample to be tested GBW03201b of table
| Element | Standard value/% | Measured value/% |
| SiO2 | 20.88 | 20.92 |
| Al2O3 | 4.48 | 4.42 |
| Fe2O3 | 2.64 | 2.69 |
| CaO | 62.76 | 62.68 |
Embodiment two
Embodiment two includes the following steps:
A, claim sample: the cement standard sample weighed respectively marked as GSB08-1533-2003, GSB08-1537, GBW03206 is each
Portion, weigh two parts marked as GBW03205b identical cement samples to be tested (cement sample marked as GBW03205b for
Buying for user is sample to be tested, needs to obtain SiO in cement by spectroscopic methodology of the invention2、Al2O3、Fe2O3With
The measured value of CaO content, referring to table 6；Cement sample marked as GBW03205b is standard sample for production and sales side
Product have been labeled with SiO in cement when dispatching from the factory sale2、Al2O3、Fe2O3With the standard value of CaO content, referring to table 4), every part
Quality is 0.1000g, and is sequentially placed in five identical silver crucibles.
B, it is sintered: being separately added into the granular sodium hydroxide of 2.0g in five silver crucibles into step A, and mix equal
It is even；Then five silver crucibles are put into 700 DEG C of Muffle furnace and are heated, melted 15~20 minutes.
C, it dissolves: the 1+1 hydrochloric acid solution of 20 mL being added into five 250 mL volumetric flasks；It is inserted into each volumetric flask
Enter a long neck funnel；Five silver crucibles are successively taken out, the end suitable for reading of corresponding long neck funnel is put into after natural cooling；It will boiling
Water is added in each crucible, after fusant falls off, is washed crucible with boiling water, is then washed crucible with 1+1 hydrochloric acid solution
And crucible cover, cleaning solution is collected together into each corresponding volumetric flask.
D, constant volume: five volumetric flasks are placed in cold bath and are cooled to room temperature；Then it plus water, shakes up, and is settled to scale,
Respectively obtain a GSB08-1533-2003 cement standard sample solution, portion GSB08-1537 cement standard sample solution, one
Part GBW03206 cement standard sample solution and two parts of GBW03205b cement testing sample solutions.
E, it draws standard curve: the obtained three parts of cement standard sample solutions of step D is successively introduced into inductive coupling etc.
In ionomer emission spectrum instrument, the instrument parameter of optimization is set, with SiO in cement standard sample solution2、Al2O3、Fe2O3、CaO
Content be abscissa, draw standard curve by ordinate of the intensity of emission spectra of Si, Al, Fe, Ca.
F, the content of oxide in cement sample to be tested is measured: by a GBW03205b cement sample to be tested in step D
Solution is introduced into inductive coupling plasma emission spectrograph, sets instrument parameter identical with step E, measures GBW03205b
The spectral intensity of Si, Al, Fe, Ca in cement testing sample solution, and according to spectral intensity and content in the standard curve of step E
Corresponding relationship check in SiO in GBW03205b cement testing sample solution2、Al2O3、Fe2O3, CaO content (referring to table 5)；
Then, repetitive operation be measured in parallel to another GBW03205b cement testing sample solution in step D.
G, it averages: according to being measured twice in step F as a result, to acquire GBW03205b cement sample to be tested respectively molten
SiO in liquid2、Al2O3、Fe2O3, CaO respectively correspond to the average value of content, referring to table 6.
Each content of material statistical form in the standard sample of 4 embodiment two of table
The parametric statistics table of each element in the standard curve of 5 embodiment two of table
| Element | Spectral line/nm | Linearly dependent coefficient |
| Si | 288.158 | 0.9999 |
| Al | 396.152 | 0.9999 |
| Fe | 238.204 | 0.9995 |
| Ca | 317.933 | 0.9996 |
The standard value of each content of material and the contrast table of measured value in 6 sample to be tested GBW03205b of table
| Element | Standard value/% | Measured value/% |
| SiO2 | 23.54 | 23.50 |
| Al2O3 | 6.60 | 6.64 |
| Fe2O3 | 3.25 | 3.21 |
| CaO | 57.25 | 57.37 |
Embodiment three
Embodiment three includes the following steps:
A, claim sample: weighing the cement standard sample each one marked as GSB08-1533-2003, GBW03205b, GBW03206 respectively
Part, weigh two parts marked as GSB08-1537 identical cement samples to be tested (cement sample marked as GSB08-1537 for
Buying for user is sample to be tested, needs to obtain SiO in cement by spectroscopic methodology of the invention2、Al2O3、Fe2O3With
The measured value of CaO content, referring to table 9；Cement sample marked as GSB08-1537 is standard sample for production and sales side
Product have been labeled with SiO in cement when dispatching from the factory sale2、Al2O3、Fe2O3With the standard value of CaO content, referring to table 7), every part
Quality is 0.1000g, and is sequentially placed in five identical silver crucibles.
B, it is sintered: being separately added into the granular sodium hydroxide of 2.0g in five silver crucibles into step A, and mix equal
It is even；Then five silver crucibles are put into 700 DEG C of Muffle furnace and are heated, melted 15~20 minutes.
C, it dissolves: the 1+1 hydrochloric acid solution of 20 mL being added into five 250 mL volumetric flasks；It is inserted into each volumetric flask
Enter a long neck funnel；Five silver crucibles are successively taken out, the end suitable for reading of corresponding long neck funnel is put into after natural cooling；It will boiling
Water is added in each crucible, after fusant falls off, is washed crucible with boiling water, is then washed crucible with 1+1 hydrochloric acid solution
And crucible cover, cleaning solution is collected together into each corresponding volumetric flask.
D, constant volume: five volumetric flasks are placed in cold bath and are cooled to room temperature；Then it plus water, shakes up, and is settled to scale,
Respectively obtain a GSB08-1533-2003 cement standard sample solution, portion GBW03205b cement standard sample solution, one
Part GBW03206 cement standard sample solution and two parts of GSB08-1537 cement testing sample solutions.
E, it draws standard curve: the obtained three parts of cement standard sample solutions of step D is successively introduced into inductive coupling etc.
In ionomer emission spectrum instrument, the instrument parameter of optimization is set, with SiO in cement standard sample solution2、Al2O3、Fe2O3、CaO
Content be abscissa, draw standard curve by ordinate of the intensity of emission spectra of Si, Al, Fe, Ca.
F, it measures the content of oxide in cement sample to be tested: a GSB08-1537 cement in step D is waited for into test sample
Product solution is introduced into inductive coupling plasma emission spectrograph, sets instrument parameter identical with step E, measures GSB08-
The spectral intensity of Si, Al, Fe, Ca in 1537 cement testing sample solutions, and according to spectral intensity in the standard curve of step E with
The corresponding relationship of content checks in SiO in GSB08-1537 cement testing sample solution2、Al2O3、Fe2O3, CaO content (referring to
Table 8)；Then, another GSB08-1537 cement testing sample solution in step D is surveyed in repetitive operation in parallel
It is fixed.
G, it averages: according to being measured twice in step F as a result, to acquire GSB08-1537 cement sample to be tested respectively molten
SiO in liquid2、Al2O3、Fe2O3, CaO respectively correspond to the average value of content, referring to table 9.
Each content of material statistical form in the standard sample of 7 embodiment three of table
The parametric statistics table of each element in the standard curve of 8 embodiment three of table
| Element | Spectral line/nm | Linearly dependent coefficient |
| Si | 288.158 | 0.9999 |
| Al | 396.152 | 0.9999 |
| Fe | 238.204 | 0.9995 |
| Ca | 317.933 | 0.9996 |
The standard value of each content of material and the contrast table of measured value in 9 sample to be tested GSB08-1537 of table
| Element | Standard value/% | Measured value/% |
| SiO2 | 16.34 | 16.30 |
| Al2O3 | 4.01 | 4.09 |
| Fe2O3 | 2.22 | 2.18 |
| CaO | 57.86 | 57.77 |
Claims (4)
1. the spectroscopic methodology of oxide content in a kind of rapid and accurate determination cement, it is characterised in that: the method includes following steps
It is rapid:
A, claim sample: weighing the cement standard sample of three parts of different labels and the cement sample to be tested of two parts of identical labels respectively, often
Part quality is 0.1000g, and is sequentially placed in five identical silver crucibles；
B, it is sintered: being separately added into the granular sodium hydroxide of 2.0g in five silver crucibles into step A, and be uniformly mixed；So
Five silver crucibles are put into 700 DEG C of Muffle furnace afterwards and are heated, are melted 15~20 minutes；
C, it dissolves: the 1+1 hydrochloric acid solution of 20 mL being added into five 250 mL volumetric flasks；One is inserted into each volumetric flask
A long neck funnel；Five silver crucibles are successively taken out, the end suitable for reading of corresponding long neck funnel is put into after natural cooling；By boiling water plus
Enter into each crucible, after fusant falls off, washs crucible with boiling water, crucible and earthenware are then washed with 1+1 hydrochloric acid solution
Crucible lid is collected cleaning solution together into each corresponding volumetric flask；
D, constant volume: five volumetric flasks are placed in cold bath and are cooled to room temperature；Then it plus water, shakes up, and is settled to scale, obtain
Three parts of cement standard sample solutions and two parts of cement testing sample solutions；
E, it draws standard curve: the obtained three parts of cement standard sample solutions of step D is successively introduced into inductively coupled plasma
In body emission spectrometer, the instrument parameter of optimization is set, with SiO in cement standard sample solution2、Al2O3、Fe2O3, CaO contains
Amount is abscissa, draws standard curve by ordinate of the intensity of emission spectra of Si, Al, Fe, Ca；
F, it measures the content of oxide in cement sample to be tested: a cement testing sample solution in step D is introduced into inductance
In coupled plasma optical emission spectrometer, identical with step E instrument parameter is set, Si in measurement cement testing sample solution,
The spectral intensity of Al, Fe, Ca, and cement is checked according to the corresponding relationship of spectral intensity and content in the standard curve of step E
SiO in testing sample solution2、Al2O3、Fe2O3, CaO content；Then, repetitive operation waits for another cement in step D
Sample solution be measured in parallel；
G, it averages: according to being measured twice in step F as a result, acquiring SiO in cement testing sample solution respectively2、Al2O3、
Fe2O3, CaO respectively correspond to the average value of content.
2. the spectroscopic methodology of oxide content in rapid and accurate determination cement according to claim 1, it is characterised in that: described
Sodium hydroxide is that analysis is pure, and hydrochloric acid solution is excellent pure grade, and water is level-one water.
3. the spectroscopic methodology of oxide content in rapid and accurate determination cement according to claim 1, it is characterised in that: described
5110 ICP-OES of model Agilent Technologies of inductive coupling plasma emission spectrograph；Set
Optimization instrument parameter: read access time be 5 s, RF power be 1200W, to stablize the time be 10 s, view mode is that radial, observation is high
Degree is 8 mm, atomization gas flow is 0.70 L/min, plasma flow amount is 12.0 L/min, secondary air amount 1.00
L/min。
4. the spectroscopic methodology of oxide content in rapid and accurate determination cement according to claim 1, it is characterised in that: described
The characteristic spectral line of Si, Al, Fe, Ca are successively selected as Si:288.158 nm, Al:396.152 nm, Fe:238.204 nm, Ca:
317.933 nm。
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| CN112710650A (en) * | 2019-12-24 | 2021-04-27 | 科之杰新材料集团有限公司 | Method for rapidly and accurately measuring main chemical component content of cement |
| CN114354521A (en) * | 2021-12-29 | 2022-04-15 | 沈阳汇晶纳米科技有限公司 | Method for testing Fe content of single-walled carbon nanotube for lithium battery |
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| 张庆华: "碱熔-电感耦合等离子体原子发射光谱（ICP-AES）法测定水泥标准物质中的氧化物含量", 《中国无机分析化学》 * |
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| CN112710650A (en) * | 2019-12-24 | 2021-04-27 | 科之杰新材料集团有限公司 | Method for rapidly and accurately measuring main chemical component content of cement |
| CN112710650B (en) * | 2019-12-24 | 2024-04-16 | 科之杰新材料集团有限公司 | Method for rapidly and accurately measuring content of main chemical components of cement |
| CN114354521A (en) * | 2021-12-29 | 2022-04-15 | 沈阳汇晶纳米科技有限公司 | Method for testing Fe content of single-walled carbon nanotube for lithium battery |
| CN114354521B (en) * | 2021-12-29 | 2024-03-22 | 沈阳汇晶纳米科技有限公司 | Method for testing Fe content of single-walled carbon nanotube for lithium battery |
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