CN103698437B - Method for quickly detecting starch coated amount in modified calcium carbonate filler through headspace gas chromatography - Google Patents
Method for quickly detecting starch coated amount in modified calcium carbonate filler through headspace gas chromatography Download PDFInfo
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- CN103698437B CN103698437B CN201410013931.5A CN201410013931A CN103698437B CN 103698437 B CN103698437 B CN 103698437B CN 201410013931 A CN201410013931 A CN 201410013931A CN 103698437 B CN103698437 B CN 103698437B
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Abstract
The invention discloses a method for quickly detecting starch coated amount in a calcium carbonate filler modified by the starch through a headspace gas chromatography. The method comprises the steps of weighing a certain amount of a calcium carbonate filler sample modified by the starch, grinding the filler sample by using a mortar, and then generating carbon dioxide by using the modified calcium carbonate filler sample which is acidized and ground by using sulfuric acid, then detecting the content of gas phase carbon dioxide by using a headspace gas chromatography, and calculating the content of calcium carbonate in the modified calcium carbonate filler according to the content of the carbon dioxide. A total mass of the modified calcium carbonate filler sample is deducted by the mass of the calcium carbonate to obtain mass of the starch coating the surface of the calcium carbonate filler. The method is quick, accurate, good in reproducibility and easy to operate. The detection method is applied to a preparation process of the modified calcium carbonate filler in a papermaking enterprise; the detection method is capable of effectively monitoring loss amount of the starch in the preparation process of the modified calcium carbonate filler and a modification effect of the calcium carbonate filler and ensuring quality of the modified calcium carbonate filler, normal operation of a papermaking machine and stability of quality of final products.
Description
Technical field
The present invention relates to field of papermaking, particularly the assay method of starch covering amount in a kind of modified calcium carbonate filler.
Background technology
In paper industry, add in paper pulp and fill out mineral filler and have a long history.Save plant fiber material owing to having, improve paper pulp drainage rate, reduce the advantages such as Dryer Section of Paper Machine energy consumption, add to fill out obtain great development in paper industry.In current paper industry raw material composition, filler is only second to vegetable fibre, accounts for the 2nd, is about 10%, and still in continuous rising.Wherein, due in, the development of alkaline paper-making, calcium carbonate is as a kind of alkaline filler, and it has pH value buffer action, and before making applying tackifier, the pH value of slurries is stabilized within the scope of the optimal pH of 7.5-8.0; The requirement of coating binder is reduced, and can save the advantages such as the expense of tackifier, the application increase of pearl filler is more remarkable.
But along with the interpolation of pearl filler, some problems also produce thereupon, the strength character as paper declines, sizing efficiency variation, the wire-cloth lost of life, printing in easily there is hair and powder dropping phenomenon etc.In order to overcome above-mentioned defect, need to carry out modification to pearl filler.Starch due to have cost low, easily coated be bonded to filling surface, with the fiber advantage such as have good bonding properties, clad not soluble, become most application potential pearl filler modifier.Up to now, have developed the method for many starch coating modification pearl fillers, as starch gelatinization modification, starch/fatty acid chelating reaction etc.Starch conversion pearl filler, not only require starch at pearl filler surface deposition many, and to pearl filler coated completely.Wherein, the starch covering amount on pearl filler surface is an important indicator of evaluation starch modified effect.
At present, there is not been reported how to measure the starch covering amount on pearl filler surface.If use the standard method of starch test, as Iodine colorimetry, polarimetry, acid-hydrolysis method and enzyme hydrolysis method (mensuration of starch " in the GB/T 5009.9-2008 food ", " in GB/T 5514-2008 grain and oil detection grain, oil plant, content of starch measures ") etc., then also exist or need that sample size is large or accuracy is lower or the problem such as complex operation.The rapid assay methods that exploitation has a pearl filler surface starch covering amount of high accuracy for control on producing the modification quality of pearl filler, the normal operation of paper machine and quality of paper products stability significant.
Summary of the invention
The object of the present invention is to provide a kind of assay method of modified calcium carbonate filler starch covering amount.The method has the advantages such as measurement result accuracy is high, simple to operate, measuring speed is fast.
For achieving the above object, the present invention adopts following technical scheme: with the calcium carbonate in sulfuric acid acidation modified calcium carbonate filler sample, produce carbon dioxide, then measure the generation of carbon dioxide by headspace gas chromatography method, thus calculate the content of calcium carbonate in modified calcium carbonate filler sample.The quality of modified calcium carbonate packing samples gross mass deduction calcium carbonate, be coated on the starch quality on pearl filler surface.Specifically comprise the following steps:
1) preparation of samples: take 5-10 gram of modified calcium carbonate packing samples and be placed in mortar and grind 5-10 minute.
2) sample preparation: the modified calcium carbonate packing samples taken after the 0.1-1.5 gram of grinding obtained in the step 1) of absolute dry mass is placed in ml headspace bottle, then stick to the modified calcium carbonate filler on ml headspace bottle wall with distilled water rinse, and coordinate aluminium lid ml headspace bottle to be sealed with teflon/butyl rubber pad.The sulfuric acid solution that 8-12mL concentration is 1-4mol/L is added again with syringe.Finally the ml headspace bottle being mounted with modified calcium carbonate filler is carried out ultrasonic process.
3) sample detection: step 2 will be housed) ml headspace bottle of modified calcium carbonate filler that obtains puts into headspace autosampler, at temperature 60-80 DEG C after constant temperature 10-20 minute, with the gas chromatograph being equipped with thermal conductivity detector (TCD), the carbon dioxide content in ml headspace bottle is detected, and record gas chromatography response peak area of signal value A
0.
4) foundation of typical curve: the sodium carbonate liquor of preparation 5-9 variable concentrations, and according to step 2) prepare modified calcium carbonate filler test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value by step 3).Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value:
In formula, A-gas chromatography response peak area of signal value;
The amount of substance of n-carbonate, μm ol;
K-slope;
B-intercept;
5) in modified calcium carbonate filler sample, starch covering amount calculates: according to step 2) absolute dry mass of the modified calcium carbonate filler sample that takes, step 3) measure the typical curve equation of gas chromatography response peak area of signal value and the step 4) acquisition obtained, starch quality degree S calculated as described below in formulae discovery modified calcium carbonate filler sample
In formula, starch quality degree in S-modified calcium carbonate filler sample, %;
The modified calcium carbonate filler sample mass of m-take, g;
A
0the gas chromatography response peak area of signal value of-test modified calcium carbonate filler sample.
The preferred capacity of above-mentioned ml headspace bottle is 20mL ml headspace bottle, the sulfuric acid solution of above-mentioned sulfuric acid solution preferred volume to be 10mL concentration be 2mol/L.
Above-mentioned steps 3) sample detection time: step 2 will be housed) ml headspace bottle of modified calcium carbonate filler that obtains puts into headspace autosampler, at preferable temperature 70 DEG C, constant temperature, time are preferably after 10 minutes, and the gas chromatograph being equipped with thermal conductivity detector (TCD) detects the carbon dioxide content in ml headspace bottle.
4 of above-mentioned steps) the setting up of typical curve time: the preferably sodium carbonate liquor of preparation 7 variable concentrations, and according to step 2) prepare modified calcium carbonate filler test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value according to step 3); Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value.
Above-mentioned head-space sampler operating conditions: equilibrium temperature 70 DEG C, equilibration time 10 minutes; Vibration condition is set to intense oscillations; Sample bottle nitrogen pressurization, 10 seconds pressing times; 15 seconds sample loop filling times, 6 seconds loop balance time; 10 seconds switching time of valve.Gas chromatography operating conditions: capillary chromatographic column model is DP-5, J & W Scientific, and its bore is 0.32mm, and thickness of thin layer is 0.25 μm, and length is 30m; Capillary chromatography column temperature 40 DEG C, injector temperature 120 DEG C; Carrier gas is nitrogen, flow velocity 1 ~ 4mL/min.Thermal conductivity detector (TCD) operating conditions: detector temperature is 220 DEG C; Carrier gas is hydrogen, and flow velocity is 10 ~ 20mL/min; Bridge electric current is 180 ~ 200mA.
The starch covering amount of described test modified calcium carbonate filler sample comprises all types of modified calcium carbonate filler, preferably as the modified calcium carbonate filler after starch coating modification such as ground chalk, precipitated calcium carbonate, gel calcium carbonate, activated Calcium carbonate, crystal calcium carbonate.
Described rinse ml headspace bottle distilled water used preferably adopts the distilled water not being dissolved with carbon dioxide of brand-new; And the distilled water of preferred 4mL amount.
In Sample Preparation Procedure, the ml headspace bottle that modified calcium carbonate filler sample is housed carries out ultrasonic process, more than 5 minutes preferred process time.
Described when preparing sodium carbonate standard solution, the carbonate concentration of tested modified calcium carbonate filler sample is within the concentration range of sodium carbonate standard solution.
Measuring method of the present invention is applied to pulping and paper-making field.
The present invention has following advantage and disadvantage relative to prior art:
(1) in headspace gas chromatography measurement modified calcium carbonate filler of the present invention, the method for starch covering amount has simple to operate, and measuring speed is fast, the advantage that accuracy is high.
(2) in headspace gas chromatography measurement modified calcium carbonate filler of the present invention, the method for starch covering amount can be directly used in commercial measurement, is conducive to the stability of producing the modified effect of control pearl filler, the normal operation of paper machine and improving quality of paper products.
Accompanying drawing explanation
Fig. 1 is the headspace gas chromatography figure of carbon dioxide in embodiment one.
Fig. 2 is the canonical plotting of preparation in embodiment one.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, be clearly and completely described below to the technical scheme in the embodiment of the present invention, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment one
1) take about 5 grams of modified calcium carbonate packing samples (taking from Jinjiang, Fujian Province You Lanfa Paper Co., Ltd) and be placed in mortar grinding 5 minutes.
2) the modified calcium carbonate packing samples taken after 0.6769 gram (in absolute dry mass) grinding is placed in the ml headspace bottle of 20mL, then stick to the modified calcium carbonate filler on ml headspace bottle wall with the rinse of 4mL distilled water, and coordinate aluminium lid ml headspace bottle to be sealed with teflon/butyl rubber pad.The sulfuric acid solution that 10mL concentration is 2mol/L is added again with syringe.Finally the ml headspace bottle being mounted with modified calcium carbonate filler is carried out ultrasonic process more than 5 minutes.
3) by after ultrasonic process, step 2 is housed) ml headspace bottle of modified calcium carbonate filler sample that obtains puts into headspace autosampler, under temperature 70 C, constant temperature is after 10 minutes, gas chromatograph (pyroconductivity detecting device) detects the carbon dioxide content in ml headspace bottle, and records gas chromatography response peak area of signal value A
0=1864.3.
4) prepare the sodium carbonate liquor of 7 variable concentrations, be respectively: 0mmol/L, 4mmol/L, 8mmol/L, 12mmol/L, 16mmol/L, 20mmol/L, 24mmol/L.According to step 2) prepare test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value according to step 3).Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value:
In formula, A-gas chromatography response peak area of signal value;
The amount of substance of n-carbonate, μm ol;
5) modified calcium carbonate filler sample starch covering amount calculates: according to step 2) take the absolute dry mass (m=0.6769 gram) of modified calcium carbonate filler sample, step 3) measures the gas chromatography response peak area of signal value (A obtained
0=1864.3) and step 4) obtain typical curve equation (
), the calcium carbonate mass percentage content S calculated as described below in formulae discovery paper samples,
Therefore, in modified calcium carbonate filler sample, the mass percentage content of starch is 10.07%.These data match by the data that acid-hydrolysis method measures with by the national standard mensuration of starch " in the GB/T 5009.9-2008 food ", illustrate that method of testing of the present invention is correctly reliable.
Embodiment two
1) take about 8 grams of modified calcium carbonate packing samples (take from laboratory and prepare sample) and be placed in mortar grinding 10 minutes.
2) the modified calcium carbonate packing samples taken after 0.5902 gram (in absolute dry mass) grinding is placed in the ml headspace bottle of 20mL, then stick to the modified calcium carbonate filler on ml headspace bottle wall with the rinse of 4mL distilled water, and coordinate aluminium lid ml headspace bottle to be sealed with teflon/butyl rubber pad.The sulfuric acid solution that 10mL concentration is 2mol/L is added again with syringe.Finally the ml headspace bottle being mounted with modified calcium carbonate filler is carried out ultrasonic process more than 5 minutes.
3) by after ultrasonic process, step 2 is housed) ml headspace bottle of modified calcium carbonate filler sample that obtains puts into headspace autosampler, under temperature 70 C, constant temperature is after 10 minutes, gas chromatograph (pyroconductivity detecting device) detects the carbon dioxide content in ml headspace bottle, and records gas chromatography response peak area of signal value A
0=1566.1.
4) prepare the sodium carbonate liquor of 7 variable concentrations, be respectively: 0mmol/L, 4mmol/L, 8mmol/L, 12mmol/L, 16mmol/L, 20mmol/L, 24mmol/L.According to step 2) prepare test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value according to step 3).Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value:
In formula, A-gas chromatography response peak area of signal value;
The amount of substance of n-carbonate, μm ol;
5) modified calcium carbonate filler sample starch covering amount calculates: according to step 2) take the absolute dry mass (m=0.5902 gram) of modified calcium carbonate filler sample, step 3) measures the gas chromatography response peak area of signal value (A obtained
0=1566.1) and step 4) obtain typical curve equation (
), the calcium carbonate mass percentage content S calculated as described below in formulae discovery paper samples,
Therefore, in modified calcium carbonate filler sample, the mass percentage content of starch is 13.34%.These data match by the data that acid-hydrolysis method measures with by the national standard mensuration of starch " in the GB/T 5009.9-2008 food ", illustrate that method of testing of the present invention is correctly reliable.
Embodiment three
1) take about 5 grams of modified calcium carbonate packing samples (taking from Fujian Xiyuan Paper Co., Ltd.) and be placed in mortar grinding 6 minutes.
2) the modified calcium carbonate packing samples taken after 0.6201 gram (in absolute dry mass) grinding is placed in the ml headspace bottle of 20mL, then stick to the modified calcium carbonate filler on ml headspace bottle wall with the rinse of 4mL distilled water, and coordinate aluminium lid ml headspace bottle to be sealed with teflon/butyl rubber pad.The sulfuric acid solution that 10mL concentration is 2mol/L is added again with syringe.Finally the ml headspace bottle being mounted with modified calcium carbonate filler is carried out ultrasonic process more than 5 minutes.
3) by after ultrasonic process, step 2 is housed) ml headspace bottle of modified calcium carbonate filler sample that obtains puts into headspace autosampler, under temperature 70 C, constant temperature is after 10 minutes, gas chromatograph (pyroconductivity detecting device) detects the carbon dioxide content in ml headspace bottle, and records gas chromatography response peak area of signal value A
0=1682.8.
4) prepare the sodium carbonate liquor of 7 variable concentrations, be respectively: 0mmol/L, 4mmol/L, 8mmol/L, 12mmol/L, 16mmol/L, 20mmol/L, 24mmol/L.According to step 2) prepare test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value according to step 3).Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value:
In formula, A-gas chromatography response peak area of signal value;
The amount of substance of n-carbonate, μm ol;
5) modified calcium carbonate filler sample starch covering amount calculates: according to step 2) take the absolute dry mass (m=0.6201 gram) of modified calcium carbonate filler sample, step 3) measures the gas chromatography response peak area of signal value (A obtained
0=1682.8) and step 4) obtain typical curve equation (
), the calcium carbonate mass percentage content S calculated as described below in formulae discovery paper samples,
Therefore, in modified calcium carbonate filler sample, the mass percentage content of starch is 11.38%.These data match by the data that acid-hydrolysis method measures with by the national standard mensuration of starch " in the GB/T 5009.9-2008 food ", illustrate that method of testing of the present invention is correctly reliable.
The headspace gas chromatography measuring condition of above-described embodiment is all: head-space sampler operating conditions: equilibrium temperature 70 DEG C, equilibration time 10 minutes; Vibration condition is set to intense oscillations; Sample bottle nitrogen pressurization, 10 seconds pressing times; 15 seconds sample loop filling times, 6 seconds loop balance time; 10 seconds switching time of valve.Gas chromatography operating conditions: capillary chromatographic column model is DP-5, J & W Scientific, and its bore is 0.32mm, and thickness of thin layer is 0.25 μm, and length is 30m; Capillary chromatography column temperature 40 DEG C, injector temperature 120 DEG C; Carrier gas is nitrogen, flow velocity 1 ~ 4mL/min.Thermal conductivity detector (TCD) operating conditions: detector temperature is 220 DEG C; Carrier gas is hydrogen, and flow velocity is 10 ~ 20mL/min; Bridge electric current is 180 ~ 200mA.
Claims (6)
1. a modified calcium carbonate filler starch covering amount headspace gas chromatography rapid test method, comprises the following steps:
1) preparation of samples: the modified calcium carbonate packing samples taking 5-10 gram is placed in mortar and grinds 5-10 minute;
2) sample preparation: the modified calcium carbonate packing samples taken after the 0.1-1.5 gram of grinding obtained in the step 1) of absolute dry mass is placed in ml headspace bottle, then stick to the modified calcium carbonate filler on ml headspace bottle wall with distilled water rinse, and coordinate aluminium lid ml headspace bottle to be sealed with teflon/butyl rubber pad; The sulfuric acid solution that 8-12mL concentration is 1-4mol/L is added again with syringe; Finally the ml headspace bottle being mounted with modified calcium carbonate filler is carried out ultrasonic process;
3) sample detection: step 2 will be housed) ml headspace bottle of modified calcium carbonate filler that obtains puts into headspace autosampler, at temperature 60-80 DEG C after constant temperature 10-20 minute, the gas chromatograph being equipped with thermal conductivity detector (TCD) detects the carbon dioxide content in ml headspace bottle, and records gas chromatography response peak area of signal value A
0; Wherein, head-space sampler operating conditions is: equilibrium temperature 70 DEG C, equilibration time 10 minutes, and vibration condition is set to intense oscillations, sample bottle nitrogen pressurization, 10 seconds pressing times, 15 seconds sample loop filling times, 6 seconds loop balance time, 10 seconds switching time of valve; Gas chromatography operating conditions is: capillary chromatographic column model is DP-5, J & W Scientific, and its bore is 0.32mm, thickness of thin layer is 0.25 μm, and length is 30m, capillary chromatography column temperature 40 DEG C, injector temperature 120 DEG C, carrier gas is nitrogen, flow velocity 1 ~ 4mL/min; Thermal conductivity detector (TCD) operating conditions: detector temperature is 220 DEG C, carrier gas is hydrogen, and flow velocity is 10 ~ 20mL/min, and bridge electric current is 180 ~ 200mA;
4) foundation of typical curve: the sodium carbonate liquor of preparation 5-9 variable concentrations, and according to step 2) prepare modified calcium carbonate filler test samples, detect carbon dioxide gas phase chromatogram response peak area of signal value according to step 3); Linear fit is utilized to set up the typical curve of relation between carbonate content and gas chromatography response peak area of signal value:
In formula, A-gas chromatography response peak area of signal value;
The amount of substance of n-carbonate, μm ol;
K-slope;
B-intercept;
5) in modified calcium carbonate filler sample, starch covering amount calculates: according to step 2) absolute dry mass of the modified calcium carbonate filler sample that takes, step 3) measure the typical curve equation of gas chromatography response peak area of signal value and the step 4) acquisition obtained, calcium carbonate mass percentage content S calculated as described below in formulae discovery modified calcium carbonate filler sample
In formula, starch quality degree in S-modified calcium carbonate filler sample, %;
The modified calcium carbonate filler sample mass of m-take, g;
A
0the gas chromatography response peak area of signal value of-test modified calcium carbonate filler sample.
2. method according to claim 1, is characterized in that, described modified calcium carbonate filler is ground chalk or precipitated calcium carbonate.
3. method according to claim 1 and 2, is characterized in that, rinse ml headspace bottle distilled water used adopts the distilled water not being dissolved with carbon dioxide of brand-new.
4. method according to claim 1 and 2, is characterized in that, in Sample Preparation Procedure, the ml headspace bottle that modified calcium carbonate filler sample is housed carries out ultrasonic process more than 5 minutes.
5. method according to claim 1 and 2, is characterized in that, during preparation sodium carbonate standard solution, the carbonate concentration of tested modified calcium carbonate filler sample is within the concentration range of sodium carbonate standard solution.
6. the application of the arbitrary described assay method of claim 1-5, it is characterized in that, described assay method is applied to pulping and paper-making field.
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| CN107255678B (en) * | 2017-05-11 | 2020-02-18 | 华南理工大学 | Method for accurately determining content of calcium carbonate in paper by utilizing headspace gas chromatography |
| RU2701868C1 (en) * | 2019-01-15 | 2019-10-02 | Общество С Ограниченной Ответственностью Научно-Производственное Предприятие "Экохимприбор" | Nitrate chalk pulp analyzer |
| CN112432916A (en) * | 2020-11-10 | 2021-03-02 | 青岛海关技术中心 | Calcium carbonate powder chemical examination and identification method and commodity classification application |
| CN114252313A (en) * | 2021-12-06 | 2022-03-29 | 贵州民族大学 | Method for rapidly analyzing content of barium sulfate in barite ore |
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| CN103018359B (en) * | 2012-11-30 | 2014-06-11 | 华南理工大学 | Method for measuring content of oxalic acid in food or vegetables |
| CN103217501B (en) * | 2013-03-29 | 2015-02-18 | 华南理工大学 | Method for determining carbon dioxide content in carbonated beverage |
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