CN109297853A - A method of for automatically detecting content of carbon black in rubber - Google Patents
A method of for automatically detecting content of carbon black in rubber Download PDFInfo
- Publication number
- CN109297853A CN109297853A CN201810959092.4A CN201810959092A CN109297853A CN 109297853 A CN109297853 A CN 109297853A CN 201810959092 A CN201810959092 A CN 201810959092A CN 109297853 A CN109297853 A CN 109297853A
- Authority
- CN
- China
- Prior art keywords
- crucible
- interface
- thermogravimetric
- thermogravimetric detector
- test software
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses a kind of method for automatically detecting content of carbon black in rubber, this method is realized by following steps: 1), and the preparation stage；2), baseline test；3), sample test；4), data are analyzed: being opened Data Analysis Software, clicked and open, selection needs the data analyzed；The corresponding weight loss of 500 DEG C in curve~800 DEG C temperature is marked, content of carbon black in rubber product is obtained.The present invention is by using thermogravimetric detector and the method detected with its mating test software to the content of carbon black in rubber, the process for realizing full-automatic detection carbon black, to effectively reduce testing cost, it is time saving and energy saving, simultaneously can quickly obtain content of carbon black in rubber product, quality control, raw material control, in terms of be of great importance.
Description
Technical field
The invention belongs to content of carbon black detection technique fields, and in particular to one kind contains for automatically detecting carbon black in rubber
The method of amount.
Background technique
Important antistatic agent, reinforcing agent and filler of the carbon black as rubber product, can effectively improve the physics of rubber
Performance, mechanical performance etc.；Carbon black is added in rubber product, it is possible to reduce the dosage of rubber, the function of improving rubber product are special
Property, to prolong its service life.
Existing content of carbon black test method, is mainly tested with tube type resistance furnace, complex steps, it is time-consuming compared with
It is long, test the disadvantages of not intuitive；When containing the pyrolytics fillers such as calcium carbonate in rubber product, it can not accurately obtain carbon black and contain
Amount, and easily obscure in rubber product decompose carbon with it is carbon black-filled.
Summary of the invention
In view of this, the main purpose of the present invention is to provide a kind of for automatically detecting the side of content of carbon black in rubber
Method, solve in the prior art complex steps, test it is not intuitive the problems such as.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows: it is a kind of for automatically detecting in rubber
The method of content of carbon black, this method are realized by following steps:
Step 1, the preparation stage
Check that nitrogen cylinder pressure reducing valve pressure ensures that flow is normal；The temperature of thermogravimetric detector connection water bath with thermostatic control is set；It beats
Thermogravimetric detector test software is opened, thermogravimetric detector starts to preheat, and shows and stablizes to the quality in thermogravimetric detector, i.e., balance is small
It does not beat in the 10s of third position after several points, preheating is completed；Preparing quality is that m1 rubber sample is spare.
Step 2, baseline test
Put crucible；Sample holder is risen by the rising button on thermogravimetric detector panel, opens the bell above bracket, is used
Empty crucible is put on bracket by tweezers, and crucible is made to be in the centre of bracket, by the declines button on thermogravimetric detector panel, branch
Frame decline playback, then cover the bell above bracket；
Newly-built test method；It is alumina crucible that crucible type used, which is arranged, at the interface of thermogravimetric detector test software,
Measurement type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature program(me) is set by Four-stage Method at the interface of thermogravimetric detector test software, and is adjusted
The flow for protecting nitrogen is 20mL/min, after confirming nitrogen flow and state, is clicked at the interface of thermogravimetric detector test software
It resets, then clicks and start to measure baseline；
The Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 650 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 300 DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 850 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 30 DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check letter
Number, after empty quality is stablized, then click " clearing is exited "；" rising " button pressed on thermogravimetric detector panel again rises sample
Product bracket opens the bell above bracket, the crucible on bracket is removed, and the quality described in tweezers clamping step 1 is m1
Rubber to be detected is placed in crucible, then crucible is returned to bracket middle, presses " decline " button on thermogravimetric detector panel,
Bracket decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, chooses previous step " baseline is completed ",
Start to load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, is filled in
Sample number into spectrum, sample ID, sample quality save document location；
Start to measure: the interface of click thermogravimetric detector test software starts to test, and instrument can start to automatically analyze, point
Data can automatically save after the completion of analysis.
Step 4, data are analyzed
Data Analysis Software is opened, is clicked " opening ", selection needs the data analyzed；To 500 DEG C in curve~800 DEG C temperature
It spends corresponding weight loss to be marked, obtains content of carbon black in rubber product.
Preferably, in the step 1, the pressure of the nitrogen cylinder is 0.02~0.1Mpa；The temperature of the water bath with thermostatic control
It is 33 DEG C, m1 is 5~10mg.
Compared with prior art, the present invention is by using thermogravimetric detector and with its mating test software to charcoal in rubber
The method that black content is detected, the process for realizing full-automatic detection carbon black save to effectively reduce testing cost
Shi Shengli, while can quickly obtain content of carbon black in rubber product, quality control, raw material control, in terms of
It is of great importance.
Detailed description of the invention
Fig. 1 is the thermal gravimetric analysis curve figure that the embodiment of the present invention obtains.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
A kind of method for automatically detecting content of carbon black in rubber provided in an embodiment of the present invention, this method by with
Lower step is realized:
Step 1, the preparation stage
Check that nitrogen cylinder pressure reducing valve pressure ensures that flow is normal；The temperature of thermogravimetric detector connection water bath with thermostatic control is set；It beats
Thermogravimetric detector test software is opened, thermogravimetric detector starts to preheat, and shows and stablizes to the quality in thermogravimetric detector, i.e., balance is small
It does not beat in the 10s of third position after several points, preheating is completed；Preparing quality is that m1 rubber sample is spare；
Wherein, the pressure of nitrogen cylinder is 0.02~0.1Mpa；The temperature of the water bath with thermostatic control is 33 DEG C, and m1 is 5~10mg.
Step 2, baseline test
Put crucible；" rising " button pressed on thermogravimetric detector panel rises sample holder, opens the bell above bracket,
Empty crucible is put on bracket with tweezers, crucible is made to be in the centre of bracket, is pressed by " decline " on thermogravimetric detector panel
Button, bracket decline playback, then cover the bell above bracket；
Newly-built test method；It is alumina crucible that crucible type used, which is arranged, at the interface of thermogravimetric detector test software,
Measurement type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature program(me) is set by Four-stage Method at the interface of thermogravimetric detector test software, and is adjusted
The flow for protecting nitrogen is 20mL/min, after confirming nitrogen flow and state, is clicked at the interface of thermogravimetric detector test software
It resets, then clicks and start to measure baseline；
Wherein, Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 650 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 300 DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 850 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 30 DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check letter
Number, after empty quality is stablized, then click " clearing is exited "；" rising " button pressed on thermogravimetric detector panel again rises sample
Product bracket opens the bell above bracket, the crucible on bracket is removed, and the quality described in tweezers clamping step 1 is m1
Rubber to be detected is placed in crucible, then crucible is returned to bracket middle, presses " decline " button on thermogravimetric detector panel,
Bracket decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, chooses previous step " baseline is completed ",
Start to load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, is filled in
Sample number into spectrum, sample ID, sample quality save document location；
Start to measure: the interface of click thermogravimetric detector test software starts to test, and instrument can start to automatically analyze, point
Data can automatically save after the completion of analysis.
Step 4, data are analyzed
Data Analysis Software is opened, is clicked " opening ", selection needs the data analyzed；To 500 DEG C in curve~800 DEG C temperature
It spends corresponding weight loss to be marked, obtains content of carbon black in rubber product.
Compared with prior art, the present invention is by using thermogravimetric detector and with its mating test software to charcoal in rubber
The method that black content is detected, the process for realizing full-automatic detection carbon black save to effectively reduce testing cost
Shi Shengli, while can quickly obtain content of carbon black in rubber product, quality control, raw material control, in terms of
It is of great importance.
Embodiment 1
Step 1, the preparation stage
The pressure for checking nitrogen cylinder is 0.05Mpa to ensure that flow is normal；The connection water bath with thermostatic control of thermogravimetric detector is set
Temperature is 33 DEG C；Thermogravimetric detector test software is opened, thermogravimetric detector starts to preheat, show to the quality in thermogravimetric detector
Stablize, i.e., do not beat in the 10s of third position after balance decimal point, preheating is completed；Preparing quality is that 10mg rubber sample is spare；
Step 2, baseline test
Put crucible；Sample holder is risen by the rising button on thermogravimetric detector panel, opens the bell above bracket, is used
Empty crucible is put on bracket by tweezers, and crucible is made to be in the centre of bracket, by the declines button on thermogravimetric detector panel, branch
Frame decline playback, then cover the bell above bracket；
Newly-built test method；It is alumina crucible that crucible type used, which is arranged, at the interface of thermogravimetric detector test software,
Measurement type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature is set at the interface of thermogravimetric detector test software according to Four-stage Method shown in following table
Program, and the flow for adjusting protection nitrogen is 20mL/min, after confirming nitrogen flow and state, in thermogravimetric detector test software
Interface click " clearings ", then click start measurement baseline；
| Initial temperature | Final temperature | Heating rate | Purge gas (N2) and flow | |
| Stage 1 | 30℃ | 650℃ | 20℃/min | N2-20mL/min |
| Stage 2 | 650℃ | 300℃ | -20℃/min | N2-20mL/min |
| Stage 3 | 300℃ | 850℃ | 20℃/min | N2-20mL/min |
| Stage 4 | 850℃ | 30℃ | -20℃/min | N2-20mL/min |
Wherein, Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 650 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 300 DEG C, the warm rate that cools down is -20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 850 DEG C, the warm rate that heats up is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 30 DEG C, the warm rate that cools down is -20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check letter
Number, after empty quality is stablized, then clicks clearing and exit；" rising " button pressed on thermogravimetric detector panel again rises sample
Bracket, open bracket above bell, the crucible on bracket is removed, with tweezers clamping step 1 in quality be 10mg to
It detects rubber and is returned to bracket middle as in crucible, then by crucible, press " decline " button on thermogravimetric detector panel, branch
Frame decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, previous step is chosen to complete baseline,
It clicks and opens load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, is filled in
Sample number into spectrum, sample ID, sample quality save file；
Step 4, data are analyzed
NETZSCH Proteus Thermal Analysis Data Analysis Software is opened, is clicked " opening ", selection needs
The data of analysis；The corresponding weight loss of 500 DEG C in curve~800 DEG C temperature is marked, carbon black in rubber product is obtained and contains
Amount.
Fig. 1 is the thermal gravimetric analysis curve figure that embodiment 1 obtains, the corresponding weight loss of 500 DEG C~800 DEG C temperature from curve
It is found that content of carbon black is 40.49% in rubber product.
Embodiment 2
Step 1, the preparation stage
The pressure for checking nitrogen cylinder is 0.05Mpa to ensure that flow is normal；The connection water bath with thermostatic control of thermogravimetric detector is set
Temperature is 33 DEG C；Thermogravimetric detector test software is opened, thermogravimetric detector starts to preheat, show to the quality in thermogravimetric detector
Stablize, i.e., do not beat in the 10s of third position after balance decimal point, preheating is completed；Preparing quality is that 5mg rubber sample is spare；
Step 2, baseline test
Put crucible；" rising " button pressed on thermogravimetric detector panel rises sample holder, opens the bell above bracket,
Empty crucible is put on bracket with tweezers, crucible is made to be in the centre of bracket, is pressed by " decline " on thermogravimetric detector panel
Button, bracket decline playback, then cover the bell above bracket；
Newly-built test method；It is aluminium oxide, measurement that crucible type used, which is arranged, at the interface of thermogravimetric detector test software
Type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature is set at the interface of thermogravimetric detector test software according to Four-stage Method shown in following table
Program, and the flow for adjusting protection nitrogen is 20mL/min, after confirming nitrogen flow and state, in thermogravimetric detector test software
Interface click " clearings ", then click start measurement baseline；
| Initial temperature | Final temperature | Heating rate | Purge gas (N2) and flow | |
| Stage 1 | 30℃ | 650℃ | 20℃/min | N2-20mL/min |
| Stage 2 | 650℃ | 300℃ | -20℃/min | N2-20mL/min |
| Stage 3 | 300℃ | 850℃ | 20℃/min | N2-20mL/min |
| Stage 4 | 850℃ | 30℃ | -20℃/min | N2-20mL/min |
Wherein, Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 650 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 300 DEG C, the warm rate that cools down is -20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 850 DEG C, the warm rate that heats up is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 30 DEG C, the warm rate that cools down is -20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check letter
Number, after empty quality is stablized, then clicks clearing and exit；" rising " button pressed on thermogravimetric detector panel again rises sample
Bracket opens the bell above bracket, the crucible on bracket is removed, and is the to be checked of 5mg with the quality in tweezers clamping step 1
It surveys rubber and is returned to bracket middle as in crucible, then by crucible, press " decline " button on thermogravimetric detector panel, bracket
Decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, previous step is chosen to complete baseline,
It clicks and opens load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, is filled in
Sample number into spectrum, sample ID, sample quality save file；
Step 4, data are analyzed
NETZSCH Proteus Thermal Analysis Data Analysis Software is opened, clicks and opens, selection needs point
The data of analysis；The corresponding weight loss of 500 DEG C in curve~800 DEG C temperature is marked, content of carbon black in rubber product is obtained.
Embodiment 3
Step 1, the preparation stage
The pressure for checking nitrogen cylinder is 0.05Mpa to ensure that flow is normal；The connection water bath with thermostatic control of thermogravimetric detector is set
Temperature is 33 DEG C；Thermogravimetric detector test software is opened, thermogravimetric detector starts to preheat, show to the quality in thermogravimetric detector
Stablize, i.e., do not beat in the 10s of third position after balance decimal point, preheating is completed；Preparing quality is that 8mg rubber sample is spare.
Step 2, baseline test
Put crucible；" rising " button pressed on thermogravimetric detector panel rises sample holder, opens the bell above bracket,
Empty crucible is put on bracket with tweezers, crucible is made to be in the centre of bracket, is pressed by " decline " on thermogravimetric detector panel
Button, bracket decline playback, then cover the bell above bracket；
Newly-built test method；It is aluminium oxide, measurement that crucible type used, which is arranged, at the interface of thermogravimetric detector test software
Type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature is set at the interface of thermogravimetric detector test software according to Four-stage Method shown in following table
Program, and the flow for adjusting protection nitrogen is 20mL/min, after confirming nitrogen flow and state, in thermogravimetric detector test software
Interface click " clearings ", then click start measurement baseline；
| Initial temperature | Final temperature | Heating rate | Purge gas (N2) and flow | |
| Stage 1 | 30℃ | 650℃ | 20℃/min | N2-20mL/min |
| Stage 2 | 650℃ | 300℃ | -20℃/min | N2-20mL/min |
| Stage 3 | 300℃ | 850℃ | 20℃/min | N2-20mL/min |
| Stage 4 | 850℃ | 30℃ | -20℃/min | N2-20mL/min |
Wherein, Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 650 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 300 DEG C, the warm rate that cools down is -20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 850 DEG C, the warm rate that heats up is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature
It is 30 DEG C, the warm rate that cools down is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check letter
Number, after empty quality is stablized, then clicks clearing and exit；" rising " button pressed on thermogravimetric detector panel again rises sample
Bracket opens the bell above bracket, the crucible on bracket is removed, and is the to be checked of 8mg with the quality in tweezers clamping step 1
It surveys rubber and is returned to bracket middle as in crucible, then by crucible, press " decline " button on thermogravimetric detector panel, bracket
Decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, previous step is chosen to complete baseline,
It clicks and opens load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, is filled in
Sample number into spectrum, sample ID, sample quality save file；
Step 4, data are analyzed
NETZSCH Proteus Thermal Analysis Data Analysis Software is opened, clicks and opens, selection needs point
The data of analysis；The corresponding weight loss of 500 DEG C in curve~800 DEG C temperature is marked, content of carbon black in rubber product is obtained.
The present invention examines the content of carbon black in rubber by using thermogravimetric detector and with its mating test software
The method of survey, the process for realizing full-automatic detection carbon black, so that testing cost is effectively reduced, it is time saving and energy saving, while can
Quickly obtain content of carbon black in rubber product, quality control, raw material control, in terms of be of great importance.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (2)
1. a kind of method for automatically detecting content of carbon black in rubber, which is characterized in that this method passes through following steps reality
It is existing:
Step 1, the preparation stage
Check that nitrogen cylinder pressure reducing valve pressure ensures that flow is normal；The temperature of thermogravimetric detector connection water bath with thermostatic control is set；Open heat
Re-detection instrument test software, thermogravimetric detector start to preheat, and show and stablize to the quality in thermogravimetric detector, is i.e. balance decimal point
It does not beat in the 10s of third position afterwards, preheating is completed；Preparing quality is that m1 rubber sample is spare；
Step 2, baseline test
Put crucible；Sample holder is risen by the rising button on thermogravimetric detector panel, the bell above bracket is opened, uses tweezers
Empty crucible is put on bracket, crucible is made to be in the centre of bracket, by the declines button on thermogravimetric detector panel, under bracket
Drop playback, then cover the bell above bracket；
Newly-built test method；It is alumina crucible, measurement that crucible type used, which is arranged, at the interface of thermogravimetric detector test software
Type selection amendment, STC and thermocouple correction are to open, and weighting manner is to be manually entered；
Edit temperature program(me)；Temperature program(me) is set by Four-stage Method at the interface of thermogravimetric detector test software, and adjusts protection
The flow of nitrogen is 20mL/min, after confirming nitrogen flow and state, clicks and resets at the interface of thermogravimetric detector test software,
It clicks again and starts to measure baseline；
The Four-stage Method specifically:
First stage: being 30 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature 650
DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Second stage: being 650 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature is
300 DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Phase III: being 300 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature is
850 DEG C, heating rate is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Fourth stage: being 850 DEG C in the initial temperature of the interface of thermogravimetric detector test software setting crucible, final temperature 30
DEG C, rate of temperature fall is 20 DEG C/min, and the flow for purging nitrogen is 20mL/min；
Step 3, sample test
Setting-out product；After baseline test to be done, is clicked in diagnosis at the interface of thermogravimetric detector test software and check signal, to
After empty quality is stablized, then click " clearing is exited "；" rising " button pressed on thermogravimetric detector panel again rises sample branch
Frame opens the bell above bracket, the crucible on bracket is removed, and the quality described in tweezers clamping step 1 is m1 to be checked
It surveys rubber to be placed in crucible, then crucible is returned to bracket middle, press " decline " button on thermogravimetric detector panel, bracket
Decline playback, then cover the bell above bracket；
Load baseline；" opening " is clicked at the interface of thermogravimetric detector test software, chooses previous step " baseline is completed ", starts
Load baseline；
Setting method parameter；Amendment+sample is selected in the measurement type at the interface of thermogravimetric detector test software, fills in sample
Number, sample ID, sample quality save document location；
Start to measure: the interface of click thermogravimetric detector test software starts to test, and instrument can start to automatically analyze, and analyze
It can be automatically saved at rear data；
Step 4, data are analyzed
Data Analysis Software is opened, is clicked " opening ", selection needs the data analyzed；To 500 DEG C in curve~800 DEG C temperature pair
The weight loss answered is marked, and obtains content of carbon black in rubber product.
2. a kind of method for automatically detecting content of carbon black in rubber according to claim 1, which is characterized in that institute
It states in step 1, the pressure of the nitrogen cylinder is 0.02~0.1Mpa；The temperature of the water bath with thermostatic control be 33 DEG C, m1 be 5~
10mg。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810959092.4A CN109297853A (en) | 2018-08-22 | 2018-08-22 | A method of for automatically detecting content of carbon black in rubber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810959092.4A CN109297853A (en) | 2018-08-22 | 2018-08-22 | A method of for automatically detecting content of carbon black in rubber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109297853A true CN109297853A (en) | 2019-02-01 |
Family
ID=65165430
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810959092.4A Pending CN109297853A (en) | 2018-08-22 | 2018-08-22 | A method of for automatically detecting content of carbon black in rubber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109297853A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896419A (en) * | 2020-08-03 | 2020-11-06 | 济宁齐鲁检测技术有限公司 | Thermal weight loss detection method and system for mixture of TESPT and carbon black and application |
| CN112683722A (en) * | 2020-12-16 | 2021-04-20 | 苏州中汽检测技术服务有限公司 | Method for measuring residual carbon content of automobile oil |
| CN113567293A (en) * | 2021-07-21 | 2021-10-29 | 湖北亿纬动力有限公司 | Method for testing content of carbon nanotubes in carbon nanotube conductive slurry |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865912A (en) * | 2006-05-16 | 2006-11-22 | 南京师范大学 | Thermal analysis method for determining silicane mixture content |
| CN104237299A (en) * | 2014-08-11 | 2014-12-24 | 广东电网公司电力科学研究院 | Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator |
-
2018
- 2018-08-22 CN CN201810959092.4A patent/CN109297853A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865912A (en) * | 2006-05-16 | 2006-11-22 | 南京师范大学 | Thermal analysis method for determining silicane mixture content |
| CN104237299A (en) * | 2014-08-11 | 2014-12-24 | 广东电网公司电力科学研究院 | Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator |
Non-Patent Citations (3)
| Title |
|---|
| 王进 等: "《轨道交通橡胶弹性元件配方分析和性能试验技术》", 31 August 2013, 中国铁道出版社 * |
| 蚂蚁文库: "tg209f1安全操作规程（精编）", 《HTTPS://WWW.MAYIWENKU.COM/P-87409.HTML》 * |
| 陈志军 等: "《近代测试技术—在高分子研究中的应用》", 31 August 1998, 成都科技大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111896419A (en) * | 2020-08-03 | 2020-11-06 | 济宁齐鲁检测技术有限公司 | Thermal weight loss detection method and system for mixture of TESPT and carbon black and application |
| CN112683722A (en) * | 2020-12-16 | 2021-04-20 | 苏州中汽检测技术服务有限公司 | Method for measuring residual carbon content of automobile oil |
| CN113567293A (en) * | 2021-07-21 | 2021-10-29 | 湖北亿纬动力有限公司 | Method for testing content of carbon nanotubes in carbon nanotube conductive slurry |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109297853A (en) | A method of for automatically detecting content of carbon black in rubber | |
| EP2669655A1 (en) | Testing apparatus for testing gas permeability on thickness direction of plastic matrix | |
| EP2669656A9 (en) | Testing apparatus for testing air permeability on thickness direction of plastic matrix, and method therefor | |
| EP2832823B1 (en) | Method for blending coal, blended coal, and method for producing coke | |
| CN104237299B (en) | Measure PDMS, SiO in silicon rubber compound insulator2, ATH content thermal analysis system | |
| CN109030335A (en) | Titanium dioxide primary product weatherability evaluation method | |
| CN102914499B (en) | Method and device for detecting moisture in mixed material during sintering process | |
| CN112067663B (en) | Method and device for detecting resistivity of high-purity silicon carbide crystal | |
| Merzlikin et al. | Ultra high vacuum high precision low background setup with temperature control for thermal desorption mass spectroscopy (TDA-MS) of hydrogen in metals | |
| CN105628785A (en) | High-purity copper correction sample for glow discharge mass spectrometer and preparation method of high-purity copper correction sample | |
| EP3608941B1 (en) | Isotope ratio measurement | |
| Siddiqui et al. | Cure kinetics modeling of cyanate-ester resin system | |
| CN107543807A (en) | One kind detects TiO in high titanium valve2The method of content | |
| CN114593775A (en) | Method for obtaining heat sealing parameters of aluminum-plastic composite film | |
| JP2017206703A (en) | Rubber composition and tire | |
| CN208937547U (en) | A kind of thermal desorption gas sample injection device and system | |
| CN109580798B (en) | Method for detecting residual expanding medium in cut tobacco | |
| CN108918340A (en) | The phenolic resin of resistance to ablation pyrolytic process discharge quantity test device and test method | |
| US10054575B2 (en) | Hydrogen detector and hydrogen detection method | |
| CN113008932A (en) | Method for correcting cross-linking degree test error | |
| US20180194624A1 (en) | Gas-Loading and Packaging Method and Apparatus | |
| CN109085192A (en) | The detection method of element silicon in a kind of pig iron | |
| CN113433986B (en) | Temperature control method, oven, electronic device and readable storage medium | |
| WO2022085080A1 (en) | Hydrogen content measuring method | |
| KR101180276B1 (en) | Inverse gas chromatography data processing method for surface characterization of nanomaterials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190201 |