CN108931419B - Method for detecting activation degree of calcium carbonate powder - Google Patents
Method for detecting activation degree of calcium carbonate powder Download PDFInfo
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- CN108931419B CN108931419B CN201810791380.3A CN201810791380A CN108931419B CN 108931419 B CN108931419 B CN 108931419B CN 201810791380 A CN201810791380 A CN 201810791380A CN 108931419 B CN108931419 B CN 108931419B
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- calcium carbonate
- turbidity
- activation degree
- sample
- activation
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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
Abstract
The invention relates to the field of an activation degree detection method, in particular to a calcium carbonate powder activation degree detection method, which determines the activation degree through calcium carbonate turbidity measurement by utilizing the principle that unactivated calcium carbonate powder can be dispersed in water, the unactivated powder can be dispersed in the water to form milky turbid liquid, the more the unactivated powder is, the higher the turbidity is, and the lower the activation degree is. The detection time of the activation degree is greatly shortened, the detection cost is greatly reduced, and the detection data is timely provided for production.
Description
Technical Field
The invention relates to the technical field of methods for detecting the activation degree, in particular to a method for detecting the activation degree of calcium carbonate powder.
Background
The calcium carbonate powder is used as a filler of a macromolecular organic substance, the calcium carbonate is an inorganic substance, and if the calcium carbonate powder is filled into the macromolecular organic substance without treatment, the calcium carbonate is agglomerated in the macromolecular organic substance due to poor compatibility of the inorganic substance and the organic substance, so that the performance of a macromolecular organic substance product is affected, and the product is unqualified. The degree of activation of the activated calcium directly affects the degree of compatibility of the calcium carbonate with the high molecular organic substance.
The current method for detecting the activation degree is to use the national recommended standard (GB/T19281-2014) for measuring the activation degree of 3.19 in the calcium carbonate analysis method, and the method comprises the following steps: about 5g of sample was weighed to the nearest 0.01 g. The mixture was placed in a separatory funnel, 200mL of water was added, and the mixture was shaken repeatedly at a speed of 120 times/min for 1 min. Standing on a funnel stand for 20-30 min. After obvious layering, the precipitated calcium carbonate is put into a glass sand crucible which is dried to constant mass at the temperature of 105 +/-2 ℃ in advance, and water is removed by suction filtration. Placing in an electric heating constant temperature drying oven, drying at 105 + -2 deg.C until the quality is constant, and calculating the activation degree. However, the method has long testing time, needs 2-3 hours for each measurement, is not suitable for daily detection, and is only suitable for post analysis and product development.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for detecting the activation degree of calcium carbonate powder, which is characterized by comprising the following steps: 1) sample treatment: weighing a sample, putting the sample into a processing container, adding water, and uniformly mixing the sample with the water; magnetic stirring is carried out for 1min in a segmented mode, and the rotating speed is 500-; 2) and (3) measuring turbidity: testing the turbidity of the sample solution prepared in the step 1); 3) conversion of the activation degree: and (3) determining the activation degree according to a formula of the turbidity of the calcium carbonate and the activation degree determined in the step 2).
Further, in the step 1), a 78-1 magnetic heating stirrer is adopted for magnetic stirring, and the processing container is a beaker.
Further, the segmented magnetic stirring operation in step 1) is as follows: placing the prepared sample in the middle of a 78-1 magnetic stirrer, starting a power switch, starting a stopwatch to count down for 0.5-3min, pausing after stirring for 10-30s, rapidly moving the beaker to an edge scale mark, immediately restarting stirring for 10-40s, and then moving the beaker back to the middle till the end of time. Further, the mass ratio of the sample to water in step 1) was 1: 50.
Further, the turbidity is measured by one of spectrophotometry, visual turbidimetry and turbidimetry.
Further, the formula of the turbidity and the activation degree of the calcium carbonate is as follows:
degree of activation (Y) — 1.6847 turbidity (X) +100
The principle of the invention is as follows: by utilizing the principle that the unactivated calcium carbonate powder can be dispersed in water and the activated calcium carbonate powder cannot be dispersed in water, the unactivated powder can be dispersed in water to form milky turbid liquid, the more the unactivated powder is, the higher the turbidity is, the lower the activation degree is, and the higher the activation degree is conversely.
Determining a corresponding formula of turbidity and activation degree: the turbidity of products with different activation degrees is tested, the activation degree is synchronously measured by the measurement of the activation degree of 3.19 in the GB/T19281-2014 calcium carbonate analysis method, the activation degree of unactivated calcium carbonate is zero, a turbidity and activation degree corresponding table is made according to the data, and a curve is drawn to determine a formula.
The invention has the beneficial effects that: the activation degree is measured by adopting the method, the whole measuring process takes about 5 minutes, the detection time is greatly reduced compared with the measuring method of the national standard (GB/T19281-2014), and data can be timely provided for production; the method disclosed by the invention is operated at normal temperature in the determination process, and the GB/T19281-2014 determination method is not required to be adopted for drying the glass sand crucible and drying the sample after the test, so that the energy consumption is greatly reduced; the method is simple and convenient in process operation and strong in operability.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Samples having an activation degree of 0, 30.2. + -. 0.2%, 49.9. + -. 0.1%, 81.6. + -. 0.6% and 93.6. + -. 0.7% as measured by the GB/T19281-2014 measurement method were designated as sample 1, sample 2, sample 3, sample 4 and sample 5, respectively.
Example one
Placing a magnetic stirrer in a clean beaker, placing the magnetic stirrer and the beaker on a balance, and resetting; weighing a sample, namely adding 2.00g of calcium carbonate sample into a beaker, and accurately measuring the calcium carbonate sample to 0.01 g; pouring 100ml of water into a sample, uniformly mixing, sealing and testing; placing the prepared sample in the middle of a 78-1 magnetic heating stirrer with the set rotating speed of 500r/min, starting a power switch, starting a stopwatch to count down for 0.5min, pressing the power switch after stirring for 10s, quickly moving the beaker to an edge scale line, immediately starting the power switch, stirring for 10s, and moving the beaker back to the middle till the time is over; and testing the turbidity of the prepared sample solution by using a turbidimeter. Adopting a formula of corresponding calcium carbonate turbidity and activation degree: degree of activation (Y) — 1.6847 turbidity (X) + 100.
Samples 1-5 were tested in parallel using the method of example one.
Example two
Placing a magnetic stirrer in a clean beaker, placing the magnetic stirrer and the beaker on a balance, and resetting; weighing a sample, namely adding 2.00g of calcium carbonate sample into a beaker, and accurately measuring the calcium carbonate sample to 0.01 g; pouring 100ml of water into a sample, uniformly mixing, sealing and testing; placing the prepared sample in the middle of a 78-1 magnetic heating stirrer with the set rotating speed of 550r/min, starting a power switch, starting a stopwatch to count down for 3min, pressing the power switch after stirring for 30s, quickly moving the beaker to the edge scale mark, immediately starting the power switch, and moving the beaker back to the middle after stirring for 40s until the time is over; and testing the turbidity of the prepared sample solution by using a turbidimeter. Adopting a formula of corresponding calcium carbonate turbidity and activation degree: degree of activation (Y) — 1.6847 turbidity (X) + 100.
Samples 1-5 were tested in parallel using the method of example two.
EXAMPLE III
Placing a magnetic stirrer in a clean beaker, placing the magnetic stirrer and the beaker on a balance, and resetting; weighing a sample, namely adding 2.00g of calcium carbonate sample into a beaker, and accurately measuring the calcium carbonate sample to 0.01 g; pouring 100ml of water into a sample, uniformly mixing, sealing and testing; placing the prepared sample in the middle of a 78-1 magnetic heating stirrer with the set rotating speed of 600r/min, starting a power switch, starting a stopwatch to count down for 1min, pressing the power switch after stirring for 10s, quickly moving the beaker to the edge scale mark, immediately starting the power switch, and moving the beaker back to the middle after stirring for 20s until the time is over; and testing the turbidity of the prepared sample solution by using a turbidimeter. Adopting a formula of corresponding calcium carbonate turbidity and activation degree: degree of activation (Y) — 1.6847 turbidity (X) + 100.
Samples 1-5 were tested in parallel using the method of example three.
Example four
The turbidity of the prepared sample solution was measured spectrophotometrically by the sample preparation method of example 3. Adopting a formula of corresponding calcium carbonate turbidity and activation degree: degree of activation (Y) — 1.6847 turbidity (X) + 100.
Samples 1-5 were tested in parallel using the method of example four.
EXAMPLE five
The turbidity of the prepared sample solution was measured by visual turbidimetry using the sample preparation method of example 3. Adopting a formula of corresponding calcium carbonate turbidity and activation degree: degree of activation (Y) — 1.6847 turbidity (X) + 100.
Samples 1-5 were tested in parallel using the method of example five.
And (3) detection results:
examples one to five test results were analyzed by single factor using SPSS software, and the results are shown in the following table:
the data in the table show that the detection methods adopted in the first to fifth embodiments of the invention are all not significantly different from the data detected by the detection method adopted in the national standard (GB/T19281-2014), so that it can be shown that the accuracy of the activation degree detection of the invention is high.
Claims (3)
1. The method for detecting the activation degree of the calcium carbonate powder is characterized by comprising the following steps:
1) sample treatment: weighing a sample, putting the sample into a processing container, adding water, and shaking lightly to mix uniformly; magnetic stirring is carried out for 1min in a segmented mode, and the rotating speed is 500-; the segmented magnetic stirring operation is as follows: placing the prepared sample in the middle of a 78-1 magnetic stirrer, starting a power switch, starting a stopwatch to count down for 0.5-3min, stirring for 10-30s, then pausing, quickly moving the beaker to an edge scale mark, immediately restarting stirring for 10-40s, and then moving the beaker back to the middle till the end of time;
2) and (3) measuring turbidity: testing the turbidity of the sample solution prepared in the step 1);
3) conversion of the activation degree: determining the activation degree of the turbidity measured in the step 2) according to a formula corresponding to the turbidity of the calcium carbonate and the activation degree;
the formula of the calcium carbonate turbidity and the activation degree is as follows:
degree of activation (Y) = -1.6847 turbidity (X) + 100.
2. The method for detecting the activation degree of calcium carbonate powder according to claim 1, wherein the method comprises the following steps: the mass ratio of the sample to the water in the step 1) is 1: 50.
3. The method for detecting the activation degree of calcium carbonate powder according to claim 1, wherein the method comprises the following steps: the turbidity measurement adopts one of spectrophotometry, visual turbidimetry and turbidimetry.
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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 |
| 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 |
| CA2848366A1 (en) * | 2011-09-15 | 2013-03-21 | Multi-Chem Group, Llc | Method for selection of surfactants in well stimulation |
| 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)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
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| 填料及其改性对纸张性能的影响;万丽;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20120515(第5期);第21-26页 * |
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