CN107966381A - A kind of new method for weighing hot rolling emulsion clean level - Google Patents
A kind of new method for weighing hot rolling emulsion clean level Download PDFInfo
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- CN107966381A CN107966381A CN201710943775.6A CN201710943775A CN107966381A CN 107966381 A CN107966381 A CN 107966381A CN 201710943775 A CN201710943775 A CN 201710943775A CN 107966381 A CN107966381 A CN 107966381A
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- 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
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Abstract
The present invention is a kind of detection method, and the content of insoluble metal ion, nonmetallic substance etc. in emulsion can be effectively analyzed during emulsion use.By analyzing contrast as indexes suddenly changed in emulsion production, and analyze the surface defect caused by emulsion reason when solving production and reliability foundation is provided.
Description
Technical field
The present invention relates to a kind of new method for weighing hot rolling emulsion clean level, specifically a kind of detection and measurement
The method of emulsion emulsion clean level during aluminium rolls use itself.
Background technology
The clean level of emulsion in use influences aluminum alloy rolled surface quality on very big, hot-rolling mill production ring
Border is more severe, and metal oxide, ground sludge, air powder can all pollute emulsion；It can make emulsion droplet granularity
Increase, ESI values decline, and reduce the stability and lubricity of emulsion, cause the residue increase of rolling plate face, increase emulsion
Consumption, and emulsion it is dirty after be more prone to surface defect.Ponder deeply, analyze according to the actual requirements, utilize existing material
A kind of and new method for weighing hot rolling emulsion clean level of detection device invention.
The content of the invention
The shortcomings that in order to overcome the above-mentioned prior art, it is clean to weigh hot rolling emulsion it is an object of the invention to provide one kind
The new method of degree, can prevent, because emulsion pollution causes the unqualified of surface quality, to reduce production efficiency；Detection method letter
It is single, it is highly practical, and do not increase cost, the detection method developed on the basis of the detection of emulsion ash content, preferably embodies acid not
Molten ash content, the necessary guidance of emulsion clean level offer in order to control, can be widely used for the detection of emulsion clean level and divides
Analysis.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of new method for weighing hot rolling emulsion clean level, includes the following steps：
Step 1, by the porcelain crucible of constant weight claim standard to 0.0001g, and with same accuracy be weighed into 10g emulsions examination
Sample；
φ 9cm half, is opened middling speed quantitative filter paper and is rolled into coniform by step 2, it is cut off apart from tip 5-10mm's with scissors
Part, is buckled in the emulsion in porcelain crucible and is used as igniting core, it is covered most of emulsion specimen surface；
During the aqueous emulsification fluid samples of step 3, measure, general-purpose will be placed on equipped with the porcelain crucible of emulsification fluid samples and igniting core
On electric furnace, slow heating, control electric furnace surface temperature makes emulsification fluid samples not spill, allows water slow evaporation within 300 DEG C,
Untill filter paper until being impregnated with sample can ignite, after igniting core is impregnated with sample, ignition, burning, which proceeds to, obtains dryness charcoal
Untill when changing residue, flame height maintains 10cm or so during burning；
Step 4, to sticky or the content of wax emulsification fluid samples, burn while heated on electric furnace, after burning starts,
Electric furnace surface temperature is adjusted within 300 DEG C, makes emulsification fluid samples are unlikely to spill, is not also overflowed from porcelain crucible edge；
After step 5, sample burning, the porcelain crucible for filling residue is moved into 775 ± 25 DEG C of Muffle furnace, it is warm herein
The lower calcining of degree, until residue is changed into ashes completely；
Into after ash, Muffle furnace takes out porcelain crucible and moves into drier, cool down 50min but to 400 ± 20 DEG C for step 6, residue
To room temperature, weigh, every 3 porcelain crucibles weighing time is not more than 1.5min, is accurate to 0.0001g；
Step 7, repeat to calcine, cool down and weigh, until weighing result difference is no more than 0.0005g twice in succession
Only；
Step 8, instill 2-3 drops distilled water wetting ash content into porcelain crucible, then adds the dilute of 30mL mass concentrations 5%
Porcelain crucible, is placed on holding slightly boiling 20min on electric furnace by hydrochloric acid, is all dissolved to porcelain crucible inner wall attachment；
After step 9, dissolving resulting solution are cooled to room temperature, φ 12.5cm middling speeds quantitative filter papers and 80mL funnel mistakes are used
Filter, fully washs porcelain crucible inner wall and outflow drop, discards filtrate, folded filter paper and sediment, be put into porcelain crucible；
Porcelain crucible, be placed on universal electric furnace and to be heated to filter paper jaundice by step 10, filter paper is lighted, until the knot completely that burns
Beam, crucible is moved into 775 ± 25 DEG C of Muffle furnaces and calcines 20min, and for residue into after ash, Muffle furnace takes out porcelain but to 400 ± 20 DEG C
Crucible is moved into drier, after cooling 50min to room temperature, is weighed, and every 3 porcelain crucibles weighing time is not more than 1.5min, accurately
To 0.0001g；
Step 11, repeat to calcine, cool down and weigh, until weighing result difference is no more than 0.0005g twice in succession
Only；
Step 12, the total ash content X of sample are calculated as follows：
X (ppm)=m1*106/m0
In formula,
The weight (g) of m1-step 6 gained ash content
The weight (g) of m0-sample
Acid insoluble ash Y in step 13, sample is calculated as follows：
Y (ppm)=m2*106/m0
In formula,
The weight (g) of m2-step 10 gained ash content
The weight (g) of m0-sample.
In the step 5, calcination time keeps 1.5h, pays attention to preventing detonation in operating process, prevents flame from being rushed from burner hearth
Go out.
In the step 5, porcelain crucible is moved into when muffle furnace is relatively low, is then warming up to 775 ± 25 DEG C again.
The porcelain crucible capacity 50mL, is submerged initially in the beaker for fill dilute hydrochloric acid before use and boils 10min taking-ups, with distillation
Water washing 2-3 times, is put into Muffle furnace after drying and calcines at least 10min at 775 ± 25 DEG C, and Muffle furnace is cooled to 400 ± 20 DEG C,
Take out porcelain crucible to move into drier, after being cooled to room temperature, weigh, be accurate to 0.0001g, repeat to calcine, cool down and claim
Amount, untill weighing result difference is not more than 0.0005g twice in succession.
Sample in bottle is acutely shaken up before emulsion sampling, has real representativeness to ensure to materials；To sticky or
Content of wax sample, is previously heated to 50-60 DEG C, is sampled after shaking up.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) content of insoluble metal ion in emulsion, nonmetallic substance etc. can effectively be analyzed.
(2) do not have to individually purchase detecting instrument for this, method is simple, and general testing staff can just detect.
(3) it is the index change of analysis emulsion, solves aluminium rolled surface defect and reliability foundation is provided.
(4) detection technique cost is low, and detection method is simple, can be used analytical strong.
Embodiment
The present invention mainly utilizes existing resource, formulates a kind of assay method of Emulsion for Hot Rolling acid insoluble ash, this side
Method can be used for detecting and weighing hot rolling emulsion emulsion clean level during aluminium rolls use itself, prevent emulsion mistake
Degree pollution effect aluminothermy rolls surface quality.
The key step and content of method are as follows：
1st, instrument and reagent：Porcelain crucible -50mL or 100mL, assay balance-it is accurate to 0.0001g, universal electric furnace
(2000W, temperature controllable), Muffle furnace-can constant temperature 800 DEG C, drier (not filling drier), glass funnel 80mL, quantitative filter
Paper-φ 9cm middling speeds, quantitative filter paper-φ 12.5cm middling speeds, dilute hydrochloric acid 5%, dilute hydrochloric acid 1:4
2nd, preparation
2.1st, 50mL porcelain crucibles are immersed and fills dilute hydrochloric acid (1:4) 10min taking-ups are boiled in beaker, are washed with distilled water
2-3 times, it is put into after drying in Muffle furnace and at least 10min is calcined at 775 ± 25 DEG C, Muffle furnace is cooled to 400 ± 20 DEG C, takes out porcelain
Crucible is moved into drier, after being cooled to room temperature, is weighed, is accurate to 0.0001g.Repeat to calcine, cool down and weigh, directly
Untill the difference of weighing result twice in succession is not more than 0.0005g.
2.2nd, sample in bottle is acutely shaken up before emulsion sampling, it is to be ensured that materialsing has real representativeness.To viscous
Thick or content of wax sample needs to be previously heated to 50-60 DEG C, is sampled after shaking up.
3rd, test procedure
3.1st, standard is claimed to be weighed into 10g samples to 0.0001g, and with same accuracy the porcelain crucible of constant weight.If examination
Sample amount increases, and can use 100mL large size porcelain crucibles instead.
3.2nd, φ 9cm half are opened into middling speed quantitative filter paper and is rolled into coniform, it is cut off apart from the portion of tip 5-10mm with scissors
Point, it is buckled in the emulsion in porcelain crucible and is used as igniting core, it is covered most of specimen surface.
When the 3.3rd, measuring aqueous sample, the porcelain crucible equipped with sample and igniting core is placed on universal electric furnace, is slowly added
Heat, control electric furnace surface temperature make it not spill, allow water slow evaporation within 300 DEG C, until the filter paper for being impregnated with sample can be with
Untill ignite.After igniting core is impregnated with sample, ignition.Untill the burning of sample should proceed to when obtaining dryness carbonization residue.
Flame height maintains 10cm or so during burning.
3.4th, to sticky or the content of wax sample, burn while being heated on circuit.After burning starts, electric furnace is adjusted
Surface temperature makes sample is unlikely to spill within 300 DEG C, is not also overflowed from porcelain crucible edge.
3.5th, after sample burning, the porcelain crucible for filling residue is moved into 775 ± 25 DEG C of Muffle furnace, in this temperature
Lower calcining, until residue is changed into ashes completely (one side calcination time keeps 1.5h).Note：Pay attention to preventing in this operating process
Detonation, flame are gone out from burner hearth, if necessary, porcelain crucible can be moved into when muffle furnace is relatively low, then it is warming up to 775 again ±
25 DEG C are cooled to 400 ± 20 DEG C.
3.6th, residue is into after ash, and Muffle furnace takes out porcelain crucible and move into drier but to 400 ± 20 DEG C, and cooling 50min is extremely
After room temperature, weigh, every 3 porcelain crucibles weighing time is not more than 1.5min, is accurate to 0.0001g.
3.7th, repeat to calcine, cool down and weigh, untill weighing result difference is not more than 0.0005g twice in succession.
3.8th, 2-3 drops distilled water wetting ash content is instilled into porcelain crucible, 30mL5% dilute hydrochloric acid is then added, porcelain crucible
Holding slightly boiling 20min on electric furnace is placed on, is all dissolved to porcelain crucible inner wall attachment.
3.9th, after solution is cooled to room temperature, filtered using φ 12.5cm middling speeds quantitative filter papers and 80mL funnels, fully washing
Porcelain crucible inner wall and outflow drop, discard filtrate, careful folded filter paper and sediment, are put into porcelain crucible.
3.10th, porcelain crucible is placed on universal electric furnace and is heated to filter paper jaundice, light filter paper, be fully completed until burning,
Crucible is moved into 775 ± 25 DEG C of Muffle furnaces and calcines 20min, for residue into after ash, Muffle furnace takes out porcelain earthenware but to 400 ± 20 DEG C
Crucible is moved into drier, after cooling 50min to room temperature, is weighed, and every 3 porcelain crucibles weighing time is not more than 1.5min, is accurate to
0.0001g。
3.11st, repeat to calcine, cool down and weigh, until weighing result difference is no more than 0.0005g twice in succession
Only.
4th, calculate
4.1, the total ash content X of sample is calculated as follows：
X (ppm)=m1*106/m0
In formula,
Ash weight (g) obtained by m1-step .3.6
The weight (g) of m0-sample
4.2nd, the acid insoluble ash Y in sample is calculated as follows：
Y (ppm)=m2*106/m0
In formula,
Ash weight (g) obtained by m2-step .3.10
The weight (g) of m0-sample
5th, test error
5.1st, the constant weight error in experimentation:Porcelain crucible taken out from drier weighing during due to non-artificial factor
The error that the amount of increasing or decreasing of caused balance indicating value produces.
5.2 filter paper errors:The error that the ash content of quantitative filter paper produces in experimentation.
This experimental method minimal error is 45ppm.
6th, demarcate
Three kinds of situations need to re-scale below：For the first time using this method measure acid insoluble ash；Blank analysis result ＞
During 65ppm；During the sample to be tested data exception of measure.Scaling method：Weigh the subsidiary standard sample 10g of this method, by 3.1 to
3.11 operating procedure is tested and calculated.
7th, calibration result judges
Standard sample ash content Y≤65ppm, experiment can be normally carried out, and Y ＞ 65ppm, please go through used equipment and material
Whether intact, whether reagent configuration qualified, personnel's operation whether meet process require that.
8. precision
Values below is not to be exceeded in the difference for two results that same operator measures：Acid insoluble ash ＜ 0.0065% with
Under, repeatability 0.0010；Acid insoluble ash is between 0.0065~0.150%, repeatability 0.0010.
9th, it is repeated
Due to different experiments room there are test error, it is necessary to same sample is analyzed by this method in different experiments room,
At least two groups of blank sample test datas are provided, repeated scope is determined again after the completion of comparison data.
The present invention is a kind of detection method, can effectively be analyzed during emulsion use in emulsion insoluble metal from
The content of son, nonmetallic substance etc..By analyzing contrast as indexes suddenly changed in emulsion production, and analyze when solving production because of breast
Surface defect provides reliability foundation caused by changing liquid reason.
Claims (5)
1. a kind of new method for weighing hot rolling emulsion clean level, it is characterised in that include the following steps：
Step 1, by the porcelain crucible of constant weight claim standard to 0.0001g, and with same accuracy be weighed into 10g emulsification fluid samples；
φ 9cm half, is opened middling speed quantitative filter paper and is rolled into coniform by step 2, it is cut off apart from the part of tip 5-10mm with scissors,
It is buckled in the emulsion in porcelain crucible and is used as igniting core, it is covered most of emulsion specimen surface；
During the aqueous emulsification fluid samples of step 3, measure, universal electric furnace will be placed on equipped with the porcelain crucible of emulsification fluid samples and igniting core
On, slow heating, control electric furnace surface temperature makes emulsification fluid samples not spill, allows water slow evaporation within 300 DEG C, until
Untill being impregnated with the filter paper of sample and can ignite, after igniting core is impregnated with sample, ignition, burning proceeds to that to obtain dryness charing residual
Untill during slag, flame height maintains 10cm or so during burning；
Step 4, to sticky or the content of wax emulsification fluid samples, burn while heated on electric furnace, after burning starts, adjustment
Electric furnace surface temperature makes emulsification fluid samples are unlikely to spill within 300 DEG C, is not also overflowed from porcelain crucible edge；
After step 5, sample burning, the porcelain crucible for filling residue is moved into 775 ± 25 DEG C of Muffle furnace, at this temperature
Calcining, until residue is changed into ashes completely；
Step 6, residue are into after ash, and Muffle furnace takes out porcelain crucible and move into drier but to 400 ± 20 DEG C, cooling 50min to room
Wen Hou, weighs, and every 3 porcelain crucibles weighing time is not more than 1.5min, is accurate to 0.0001g；
Step 7, repeat to calcine, cool down and weigh, untill weighing result difference is not more than 0.0005g twice in succession；
Step 8, instill 2-3 drops distilled water wetting ash content into porcelain crucible, then adds the dilute hydrochloric acid of 30mL mass concentrations 5%,
Porcelain crucible is placed on holding slightly boiling 20min on electric furnace, is all dissolved to porcelain crucible inner wall attachment；
After step 9, dissolving resulting solution are cooled to room temperature, are filtered, filled using φ 12.5cm middling speeds quantitative filter papers and 80mL funnels
Divide washing porcelain crucible inner wall and outflow drop, discard filtrate, folded filter paper and sediment, be put into porcelain crucible；
Porcelain crucible, be placed on universal electric furnace and to be heated to filter paper jaundice by step 10, lights filter paper, will until burning is fully completed
Crucible moves into 775 ± 25 DEG C of Muffle furnaces and calcines 20min, and for residue into after ash, Muffle furnace takes out porcelain crucible but to 400 ± 20 DEG C
Move into drier, after cooling 50min to room temperature, weigh, every 3 porcelain crucibles weighing time is not more than 1.5min, is accurate to
0.0001g；
Step 11, repeat to calcine, cool down and weigh, untill weighing result difference is not more than 0.0005g twice in succession；
Step 12, the total ash content X of sample are calculated as follows：
X (ppm)=m1*106/m0
In formula,
The weight of m1-step 6 gained ash content, unit g；
The weight of m0-sample, unit g；
Acid insoluble ash Y in step 13, sample is calculated as follows：
Y (ppm)=m2*106/m0
In formula,
The weight of m2-step 10 gained ash content, unit g.
2. the new method of hot rolling emulsion clean level is weighed according to claim 1, it is characterised in that in the step 5,
Calcination time keeps 1.5h, pays attention to preventing detonation in operating process, prevents flame from being gone out from burner hearth.
3. the new method of hot rolling emulsion clean level is weighed according to claim 1, it is characterised in that in the step 5,
Porcelain crucible is moved into when muffle furnace is relatively low, is then warming up to 775 ± 25 DEG C again.
4. the new method of hot rolling emulsion clean level is weighed according to claim 1, it is characterised in that the porcelain crucible holds
50mL is measured, is submerged initially in before use in the beaker for fill dilute hydrochloric acid and boils 10min taking-ups, be washed with distilled water 2-3 times, put after drying
Enter and calcine at least 10min in Muffle furnace at 775 ± 25 DEG C, Muffle furnace is cooled to 400 ± 20 DEG C, takes out porcelain crucible and moves into drier
In, after being cooled to room temperature, weigh, be accurate to 0.0001g, repeat to calcine, cool down and weigh, until weighing knot twice in succession
Untill fruit difference is not more than 0.0005g.
5. the new method of hot rolling emulsion clean level is weighed according to claim 1, it is characterised in that before emulsion sampling
Sample in bottle is acutely shaken up, has real representativeness to ensure to materials；To sticky or content of wax sample, it is previously heated to
50-60 DEG C, it is sampled after shaking up.
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| CN201710943775.6A CN107966381A (en) | 2017-10-11 | 2017-10-11 | A kind of new method for weighing hot rolling emulsion clean level |
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Citations (4)
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| RU2283484C9 (en) * | 2005-03-28 | 2007-01-20 | Закрытое акционерное общество "Научно-производственное объединение Экрос" | Composition of standard samples for controlling error of measurements of oil products content in watery substances |
| RU2492474C1 (en) * | 2012-04-19 | 2013-09-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Забайкальский государственный университет" (ФГБОУ ВПО "ЗабГУ") | Method to determine lower calorific value of field coals |
| CN103969147A (en) * | 2014-04-17 | 2014-08-06 | 广州特种承压设备检测研究院 | Full-automatic petroleum ash determinator |
| CN106680134A (en) * | 2015-12-30 | 2017-05-17 | 奎克化学（中国）有限公司 | Method for determining iron soap content in emulsion |
-
2017
- 2017-10-11 CN CN201710943775.6A patent/CN107966381A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2283484C9 (en) * | 2005-03-28 | 2007-01-20 | Закрытое акционерное общество "Научно-производственное объединение Экрос" | Composition of standard samples for controlling error of measurements of oil products content in watery substances |
| RU2492474C1 (en) * | 2012-04-19 | 2013-09-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Забайкальский государственный университет" (ФГБОУ ВПО "ЗабГУ") | Method to determine lower calorific value of field coals |
| CN103969147A (en) * | 2014-04-17 | 2014-08-06 | 广州特种承压设备检测研究院 | Full-automatic petroleum ash determinator |
| CN106680134A (en) * | 2015-12-30 | 2017-05-17 | 奎克化学（中国）有限公司 | Method for determining iron soap content in emulsion |
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| MA...U@126.COM: "石油化工产品灰份检测", 《百度文库》 * |
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Application publication date: 20180427 |