CN108931419A - A kind of detection method of calcium carbonate powder activation grade - Google Patents
A kind of detection method of calcium carbonate powder activation grade Download PDFInfo
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- CN108931419A CN108931419A CN201810791380.3A CN201810791380A CN108931419A CN 108931419 A CN108931419 A CN 108931419A CN 201810791380 A CN201810791380 A CN 201810791380A CN 108931419 A CN108931419 A CN 108931419A
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- calcium carbonate
- activation grade
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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Abstract
The present invention relates to the detection method fields of activation grade, especially a kind of detection method of calcium carbonate powder activation grade, it can be dispersed in water using non-activated Paris white, non-activated powder will disperse the liquid for just forming milky muddiness in water, non-activated powder is more, and turbidity is higher, the lower principle of activation grade, by calcium carbonate turbidimetric analysis turbidimetry, activation grade is determined.The detection time of activation grade is substantially reduced, testing cost provides detection data to produce in time.
Description
Technical field
The present invention relates to the detection method technical field of activation grade, especially a kind of detection side of calcium carbonate powder activation grade
Method.
Background technique
Calcium carbonate powder be using quite a few macromolecule organic filler, and must be uniform as filler
It is dispersedly filled into and is filled inside object, and calcium carbonate is inorganic matter, if being filled with macromolecule organic without processing
In, due to the poor compatibility of inorganic matter and organic matter, it will lead to calcium carbonate and reunite in macromolecule organic, to influence
The performance of macromolecule organic product causes product unqualified, and is surface-treated to calcium carbonate, that is, being activated then can be with
The surface characteristic for changing calcium carbonate enables calcium carbonate to carry out with macromolecule organic good compatible, this by changing surface
The calcium carbonate of characteristic is known as calcium activated.And the activation grade of calcium activated then directly affects the calcium carbonate journey compatible with macromolecule organic
Degree.
The detection method of activation grade is using national proposed standard (GB/T 19281-2014) calcium carbonate analysis side at present
The measurement of 3.19 activation grades, this method in method are as follows: weigh about 5g sample, be accurate to 0.01g.It is placed in separatory funnel, adds 200mL
Water back and forth shakes 1min with the speed of 120 times/min.It puts down gently in standing 20min-30min on funnel stand.It is latter to obviously be layered
Secondary property by sinking calcium carbonate be put into it is pre- prior to 105 DEG C ± 2 DEG C at dry into the sintered-glass filter crucible of constant mass, filter remove
Water.It is placed in Constant Temp. Oven, in 105 DEG C of ± 2 DEG C of dryings to constant mass, calculates activation grade.But when the method is tested
Between it is long, every time measurement need 2-3 hour, be not suitable for daily detection, be suitable only for ex-post analysis use and research and development product use.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of calcium carbonate powder activation grade
Detection method, which comprises the following steps: 1) sample treatment: sample is weighed as water in process container, is added, is shaken clearly
It mixes；It is segmented magnetic agitation 1min, revolving speed 500-600r/min；2) turbidimetric analysis turbidimetry: the configured sample liquid test of step 1) is turbid
Degree；3) activation grade converts: the turbidity that step 2) measures is determined activation grade according to calcium carbonate turbidity formula corresponding with activation grade.
Further, magnetic agitation uses 78-1 magnetic heating stirrer in step 1), and process container is beaker.
Further, the segmentation magnetic agitation operation in step 1) is as follows: the sample prepared is placed 78-1 magnetic stirring apparatus
Centre opens power switch, while starting stopwatch countdown 0.5-3min, suspends after stirring 10-30s, beaker is moved to rapidly
After edge graduation mark, stirring 10-40s is restarted immediately, and be moved back to intermediate terminates to the time later.Further, in step 1) sample with
The mass ratio of water is 1:50.
Further, the measuring method that turbidimetric analysis turbidimetry uses is one in spectrophotometry, visual turbidimetry or turbidimeter method
Kind.
Further, calcium carbonate turbidity formula corresponding with activation grade are as follows:
Activation grade (Y)=- 1.6847 turbidity (X)+100
The principle of the invention are as follows: it can be dispersed in water using non-activated Paris white, and activated calcium carbonate powder is in water
In the principle that cannot disperse, non-activated powder will disperse the liquid for just forming milky muddiness in water, and non-activated powder is more,
Turbidity is higher, shows that activation grade is lower, otherwise activation grade is higher.
Turbidity determines method from the corresponding formula of activation grade: to the product test turbidity of different activation grades, synchronizing and uses GB/T
The measurement of 3.19 activation grades measures activation grade, the activation of non-activated calcium carbonate in 19281-2014 calcium carbonate analysis methods
Degree is zero, by these data creating turbidity table corresponding with activation grade, and draws curve, determines formula.
The invention has the advantages that: activation grade measurement is carried out using the present invention, whole measurement process is about 5 minutes time-consuming, phase
National standard (GB/T 19281-2014) method for measuring detection time is greatly declined, can be mentioned in time for production
For data；It operates, does not need using 19281-2014 measuring method of GB/T under normal temperature conditions in continuous mode of the present invention
Sample is dried after sintered-glass filter crucible is dried and tested, and greatly reduces energy consumption；And present invention process is easy to operate, operability
By force.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
Will by 19281-2014 measuring method of GB/T measurement post activation degree be 0,30.2 ± 0.2%, 49.9 ±
0.1%, 81.6 ± 0.6% and 93.6 ± 0.7% sample is set to sample 1, sample 2, sample 3, sample 4 and sample 5.
Embodiment one
Magnetic stir bar is placed in clean beaker, is placed on balance together with beaker, reset；Weighing sample is to burning
2.00g calcium carbonate sample is added in cup, is accurate to 0.01g；To pour into 100ml water into sample, mix, sealing is to be measured；It will match
It is to open power switch among the 78-1 magnetic heating stirrer of 500r/min, start simultaneously that good sample, which is placed in setting revolving speed,
Stopwatch countdown 0.5min presses power switch after stirring 10s, opens power supply immediately after beaker is moved to rapidly edge graduation mark
Switch, stirring to be moved back to after 10s intermediate terminates to the time；Configured sample liquid nephelometer is tested into turbidity.It is turbid using calcium carbonate
Spend formula corresponding with activation grade: activation grade (Y)=- 1.6847 turbidity (X)+100 calculates activation grade.
Sample 1-5 is all made of the method detection of embodiment one, tests twice in parallel.
Embodiment two
Magnetic stir bar is placed in clean beaker, is placed on balance together with beaker, reset；Weighing sample is to burning
2.00g calcium carbonate sample is added in cup, is accurate to 0.01g；To pour into 100ml water into sample, mix, sealing is to be measured；It will match
It is to open power switch among the 78-1 magnetic heating stirrer of 550r/min, start simultaneously that good sample, which is placed in setting revolving speed,
Stopwatch countdown 3min presses power switch after stirring 30s, beaker is moved to rapidly after edge graduation mark and opens power supply immediately and open
It closes, stirring to be moved back to after 40s intermediate terminates to the time；Configured sample liquid nephelometer is tested into turbidity.Using calcium carbonate turbidity
Formula corresponding with activation grade: activation grade (Y)=- 1.6847 turbidity (X)+100 calculates activation grade.
Sample 1-5 is all made of the method detection of embodiment two, tests twice in parallel.
Embodiment three
Magnetic stir bar is placed in clean beaker, is placed on balance together with beaker, reset；Weighing sample is to burning
2.00g calcium carbonate sample is added in cup, is accurate to 0.01g；To pour into 100ml water into sample, mix, sealing is to be measured；It will match
It is to open power switch among the 78-1 magnetic heating stirrer of 600r/min, start simultaneously that good sample, which is placed in setting revolving speed,
Stopwatch countdown 1min presses power switch after stirring 10s, beaker is moved to rapidly after edge graduation mark and opens power supply immediately and open
It closes, stirring to be moved back to after 20s intermediate terminates to the time；Configured sample liquid nephelometer is tested into turbidity.Using calcium carbonate turbidity
Formula corresponding with activation grade: activation grade (Y)=- 1.6847 turbidity (X)+100 calculates activation grade.
Sample 1-5 is all made of the method detection of embodiment three, tests twice in parallel.
Example IV
Using the sample preparation method of embodiment 3, configured sample liquid spectrophotometry is tested into turbidity.Using carbonic acid
Calcium turbidity formula corresponding with activation grade: activation grade (Y)=- 1.6847 turbidity (X)+100 calculates activation grade.
Sample 1-5 is all made of the method detection of example IV, tests twice in parallel.
Embodiment five
Using the sample preparation method of embodiment 3, the visual turbidimetry of configured sample liquid is tested into turbidity.Using carbonic acid
Calcium turbidity formula corresponding with activation grade: activation grade (Y)=- 1.6847 turbidity (X)+100 calculates activation grade.
Sample 1-5 is all made of the method detection of embodiment five, tests twice in parallel.
Testing result:
One to five testing result of embodiment carries out single factor analysis using SPSS software, as a result as shown in the table:
Data are shown in the above table, the embodiment of the present invention one to five use detection method with national standard (GB/
T19281-2014) data that the detection method used detects are without marked difference, it can be said that bright present invention detection activation grade
Accuracy it is high.
Claims (6)
1. a kind of detection method of calcium carbonate powder activation grade, which comprises the following steps:
1) sample treatment: sample is weighed as water in process container, is added, is shaken to mixed clearly even；It is segmented magnetic agitation 1min, revolving speed 500-
600r/min；
2) the configured sample liquid of step 1) turbidimetric analysis turbidimetry: is tested into turbidity；
3) activation grade converts: the turbidity that step 2) measures is determined activation grade according to calcium carbonate turbidity formula corresponding with activation grade.
2. a kind of method of quickly measurement calcium carbonate powder activation grade as described in claim 1, it is characterised in that: the step
1) magnetic agitation uses 78-1 magnetic heating stirrer in, and process container is beaker.
3. a kind of method of quickly measurement calcium carbonate powder activation grade as described in claim 1, it is characterised in that: the step
1) the segmentation magnetic agitation operation in is as follows: the sample prepared being placed among 78-1 magnetic stirring apparatus, opens power switch, together
Shi Qidong stopwatch countdown 0.5-3min suspends after stirring 10-30s, after beaker is moved to rapidly edge graduation mark, restarts immediately
10-40s is stirred, be moved back to intermediate terminates to the time later.
4. a kind of method of quickly measurement calcium carbonate powder activation grade as described in claim 1, it is characterised in that: the step
1) mass ratio of sample and water is 1:50 in.
5. a kind of detection method of calcium carbonate powder activation grade as described in claim 1, it is characterised in that: the turbidity is surveyed
Surely the measuring method used is one of spectrophotometry, visual turbidimetry or turbidimeter method.
6. a kind of detection method of calcium carbonate powder activation grade as described in claim 1, it is characterised in that: the calcium carbonate
Turbidity formula corresponding with activation grade are as follows:
Activation grade (Y)=- 1.6847 turbidity (X)+100
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| CN201810791380.3A CN108931419B (en) | 2018-07-18 | 2018-07-18 | Method for detecting activation degree of calcium carbonate powder |
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Citations (8)
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| CN103454180A (en) * | 2013-08-27 | 2013-12-18 | 陕西科技大学 | Method for measuring surface activation degree of modified powder material |
| CN106814013A (en) * | 2017-01-19 | 2017-06-09 | 国家纳米科学中心 | A kind of method based on the heterogeneous nano particle diameter of spectrum turbidity in site measurement and its coating thickness |
| CN106932352A (en) * | 2017-04-14 | 2017-07-07 | 河海大学 | A kind of method for determining activated sludge coefficient of stabilization |
| CN207423744U (en) * | 2017-11-08 | 2018-05-29 | 天津金发新材料有限公司 | A kind of measurement device of powder activation grade |
-
2018
- 2018-07-18 CN CN201810791380.3A patent/CN108931419B/en active Active
Patent Citations (8)
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|---|---|---|---|---|
| CN101187656A (en) * | 2007-12-12 | 2008-05-28 | 武汉大学 | Method for evaluating antiscaling ability based on turbidity change curve |
| CN101587054A (en) * | 2009-06-25 | 2009-11-25 | 南京林业大学 | Method for measuring first pass retention of wet end rapidly |
| CA2848366A1 (en) * | 2011-09-15 | 2013-03-21 | Multi-Chem Group, Llc | Method for selection of surfactants in well stimulation |
| CN102928478A (en) * | 2012-11-08 | 2013-02-13 | 广西华纳新材料科技有限公司 | Method for fast determining activity degrees of lime milk |
| CN103454180A (en) * | 2013-08-27 | 2013-12-18 | 陕西科技大学 | Method for measuring surface activation degree of modified powder material |
| CN106814013A (en) * | 2017-01-19 | 2017-06-09 | 国家纳米科学中心 | A kind of method based on the heterogeneous nano particle diameter of spectrum turbidity in site measurement and its coating thickness |
| CN106932352A (en) * | 2017-04-14 | 2017-07-07 | 河海大学 | A kind of method for determining activated sludge coefficient of stabilization |
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