CN108387479A - A kind of method of free silica content in detection air - Google Patents
A kind of method of free silica content in detection air Download PDFInfo
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- CN108387479A CN108387479A CN201810163143.2A CN201810163143A CN108387479A CN 108387479 A CN108387479 A CN 108387479A CN 201810163143 A CN201810163143 A CN 201810163143A CN 108387479 A CN108387479 A CN 108387479A
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Abstract
The invention discloses a kind of methods of free silica content in detection air, including：S1 sample collections, main solvent and secondary solvent are prepared；S2 sample pretreatments carry out containing miscellaneous measurement and alignment processing obtain pretreatment product；S3 is dissolved by heating, and pretreatment product and main solvent is mixed, and heating stirring obtains solidliquid mixture；Solidliquid mixture is filtered with filter paper, obtains sediment by S4 cold filtrations；Filter paper and sediment are ashed by S5 after-treatments, and secondary solvent is added and continues heating until not emitting white cigarette, then calcination obtains waste residue；S6, which is weighed, to be calculated, and weighs the quality of sediment and waste residue, the content of free silicon dioxide in air is obtained by calculation.The present invention by sample pretreatment, detect the impurity contained in sample, and corresponding impurity is directly corresponded to carry out follow-up removal of impurities processing, the operation to clean instead of original blindness, simplify the flow of removal of impurities, shorten experiment duration, reduce the harmful effect that extra removal step generates experiment, improves test accuracy.
Description
Technical field
The present invention relates to environmental monitoring technologies, more specifically, it relates to which free silicon dioxide contains in a kind of detection air
The method of amount.
Background technology
Medical research is the main mineral constituent for causing pneumoconiosis it has been proved that free silicon dioxide in industrial dust,
Therefore countries in the world today mine safety code in, to the regulation of operating environment dust in air concentration permissible value, be all with
Free silica content value in dust is foundation.China's revision in 2006《Safety regulations in coal mine》In the 739th article regulation,
The concentration of dust (total dust, respirable dust) should meet related request in air of workplace, it can be seen that dissociate in dust
The content of silica has close relationship with the occurrence and development of pneumoconiosis cancer, so grasping comprehensively and carrying out free silicon dioxide
Content monitoring, it is particularly important for the generation of effective prevention and control occupational disease.
And now for the measurement of the silica to dissociate in air, most widely used is conversion, in dust
Silicate and metal oxide, which can be dissolved in, to be heated in 250 DEG C of pyrophosphoric acid, but free silica is scarce substantially insoluble, into
And realize the separation of silica.But, more using process Program, it is complicated for operation, as Ou Yangtian moneys are published in 2015
The 34th phase of year《Enterprise's technology development monthly magazine》On paper《Coke oven engine surveys the improvement of free silicon dioxide method》In,
Just describe the shortcoming for the assay method of free silica content in air, but its a variety of suggestion for proposing compared with
For routine, effect is general, when especially carrying out removal of impurities processing during the test, needs repeatedly to instill different reaction dissolvents pair
Different impurity sources is answered repeatedly to be handled, not only complicated for operation, test period is longer, and is repeatedly often produced in processing procedure
Raw additional residual brings other impurities source, reduces the precision of experiment.Therefore it also needs to propose one kind compared to the prior art more
Easy, test period is shorter and the higher detection method of stringency of test.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide free silicon dioxide in a kind of detection air
The method of content has achieved the effect that shorten experiment duration, has improved test accuracy.
To achieve the above object, the present invention provides following technical solutions：Free silicon dioxide contains in a kind of detection air
The method of amount, includes the following steps：
S1, sample collection, solvent are prepared, and the solvent includes main solvent and secondary solvent, and the main solvent is a concentration of 85%
Pyrophosphate solution, the pair solvent include at least the first secondary solvent of the ammonium nitrate solution of a concentration of 2mol/L, by a concentration of
The sulfuric acid solution of 9mol/L and a concentration of 40% hydrofluoric acid solution composition the second secondary solvent in one kind；
S2, sample pretreatment carry out the sample obtained in S1 to contain miscellaneous measurement：Organic carbon is carried out to the sample collected in S1
Assay, when sample detection when containing organic carbon, the sample collected in S1 is ashed at 800 DEG C -900 DEG C 30min-35min,
Sulfide mineral assay is carried out to the sample collected in S1, when sample detection Containing Sulfur mineral, instills described first
Secondary solvent removes sulfide mineral, obtains pretreatment product；
S3 is dissolved by heating, and product will be pre-processed described in S2 and the main solvent mixes, and be heated to 245 DEG C -250 DEG C, persistently stirred
15min is mixed, solidliquid mixture is obtained；
S4, cold filtration filter the solidliquid mixture in S3 with filter paper, obtain sediment, and weigh the quality of the sediment；
S5, after-treatment, by S4 filter paper and sediment be ashed 30min-35min at 800 DEG C -900 DEG C, be added described second
Secondary solvent, and continue heating until not emitting white cigarette, the calcination at 900 DEG C obtains waste residue；
S6 is weighed and is calculated, and completes the quality of weighing waste residue after after-treatment, free silicon dioxide in air is obtained by calculation
Content.
Through the above technical solutions, sample is pre-processed, by detecting the impurity for determining contain in sample in advance, and
Corresponding impurity is directly corresponded to carry out follow-up removal of impurities processing, that is, has reached the flow of simplified removal of impurities, shortens experiment duration, and energy
It is enough to reduce the harmful effect that nuisance operation generates experiment in removal of impurities, improve the precision of experiment.Moreover, to impurity in pretreatment
Detection and experiment be normally carried out conflicting in not having time or step, it may be considered that be carried out at the same time, further shortening
The duration of experiment.
Further preferably：It is the first sample that the sample collected in S1, which is separated 0.1g-0.2g, remaining is the second sample
Product, first sample are used to measure the content of silica, and second sample is used to carry out to contain miscellaneous measurement in the S2.
Through the above technical solutions, sample is divided into the first sample and the second sample, to by subjects and containing miscellaneous survey
Fixed subjects separate, and the detection of measurement and magazine hence for dioxide-containing silica separately carries out, and it is extra to be avoided that
The additional effect that removal of impurities reaction dissolvent generates subjects, is further reduced the influence factor to experiment, improves test result
Precision.Further, it is provided separately due to subjects and containing miscellaneous measure object, can be tested and be carried out at the same time with both sides, into one
Step shortens the duration of experiment, when detecting corresponding impurity, just needs to carry out corresponding removal of impurities processing to subjects, if not
It detects corresponding impurity, then directly removal of impurities processing can not carried out to subjects, reach and shorten test period, short form test stream
Journey and reduction excess of solvent and operation dysgenic effect caused by experiment.
Further preferably：When second sample detection when containing organic carbon, by first sample in 800 DEG C -900 DEG C
Lower ashing 30min-35min processing, when the second sample detection Containing Sulfur mineral, in first sample instill described in
First secondary solvent, and first sample is all soaked.
Through the above technical solutions, when detection is containing organic carbon, organic carbon can be directly removed by being ashed, and detect and contain
When sulfide mineral, the first secondary solvent can be prepared when preparing secondary solvent and be completed, to remove the sulfide mineral contained；If inspection
It surveys and does not contain organic carbon and/or sulfide mineral, then can directly reduce corresponding removal step, simplify operating procedure, while also subtracting
Pollution of the reagent to sample when cleaning less, and then achieve the effect that improve the precision measured.
Further preferably：The sample acquired in the S1 is placed in 102 DEG C -108 DEG C of temperature and is dried, when dry
Between continue 2h, complete dry postcooling and be ground to room temperature, and to sample, until sample surfaces are smooth.
Through the above technical solutions, thoroughly removing moisture by dry, then sample surfaces are ground to smooth, reduction dust
Contact area between particle reduces the attachment force between dust particles and other impurities, convenient for removal of impurities.
Further preferably：When cooling in the S4, temperature is down to 40 DEG C -50 DEG C, then is by solidliquid mixture and volume
50 DEG C -80 DEG C of the distilled water of 150ml-200ml is mixed evenly.
Solidliquid mixture is diluted through the above technical solutions, hot distilled water is added, is convenient for subsequent filter operation.
Further preferably：The filter paper first carries out pickling processes, then lead to after sediment is obtained by filtration to the sediment
It crosses distilled water and washes spent pickling acid, until sediment is washed till neutrality.
Through the above technical solutions, by pickling, the metal that can be reacted with acid that may contain in sediment is removed,
And other are dissolved in the alkaline matter of acid, improve the purity of silica in sediment.
Further preferably：When the pickling processes, rinsed using the hydrochloric acid solution of a concentration of 0.1mol/L, and to sediment
3-5 times.
Through the above technical solutions, after carrying out pickling using hydrochloric acid, the component part in sediment is substantially by insoluble in acid
Substance and silica composition, purity are relatively high.
Further preferably：When the second secondary solvent being added in the S5, the sulfuric acid that a concentration of 9mol/L of 5-8 drops is first added is molten
The sediment by ashing is all soaked, adds the hydrofluoric acid of 5ml-10ml a concentration of 40% by liquid.
Silica is dissolved through the above technical solutions, the second secondary solvent is added, and remaining is insoluble in acid
Impurity, and then can obtain the content of silica.
Further preferably：When detecting free silica content in air, it is provided with blank control group, the blank pair
The step of passing through with first sample according to group operating procedure is identical.
Through the above technical solutions, setting blank control group, and operating procedure is identical as the first sample, and then can be complete
After all operations, test result is improved as the corrected parameter of this experiment by the variation to weight before and after blank control group
Precision, eliminate the harmful effect that the factor that some are difficult to observe by is brought.
In conclusion the invention has the advantages that：By to sample pretreatment, detect to contain in sample
Impurity, and corresponding impurity is directly corresponded to carry out follow-up removal of impurities processing, no impurity can save corresponding removal step,
The flow of simplified removal of impurities is reached, has reduced step, and can reduce and extra experiment be generated not in removal of impurities except miscellaneous operation
Good influence improves the precision of experiment, simultaneously because the operation of checked for impurities can be synchronous with the experiment of silicon dioxide content test
It carries out, additional test period will not be increased, therefore can also shorten the duration of experiment when reducing step.
Specific implementation mode
With reference to embodiment, the present invention will be described in detail.
Embodiment 1：A kind of method of free silica content in detection air, including the step of it is as follows：S1, sample are adopted
Collection, solvent are prepared
When sample collection, using the dust in the filter membrane big flow acquisition air of diameter 75mm, the sample of acquisition is placed in 102 DEG C
It is dried in temperature, drying time continues 2h, completes dry postcooling and is ground to room temperature and to sample, until sample table
Face is smooth.Collected dust is directly divided into totally two parts of the first sample and the second sample, the first sample therein is as experiment
Sample, to carry out the detection of free silica content in air, the second sample is as test sample, for detecting acquisition
The impurity contained in sample, wherein the quality of the first sample is 0.12g；
When solvent is prepared, need to prepare main solvent and secondary solvent, the phosphoric acid solution that main solvent is a concentration of 85% is heated to
Until 250 DEG C of not bubblings, standing waits for its cooling, and is stored in spare in reagent bottle.Secondary solvent includes the first secondary solvent and second
Secondary solvent, the first secondary solvent are 2mol/L ammonium nitrate solutions, and the second secondary solvent includes the sulfuric acid solution of a concentration of 9mol/L and dense
Degree is 40% hydrofluoric acid solution, and the second secondary solvent prepares spare in advance, if need to prepare the first pair solvent simultaneously, then by
Sulfide mineral whether is detected to determine in subsequent sample pretreatment.
S2, sample pretreatment
Second sample is divided into two parts, conventional dichromic acid can be used for detecting whether contain organic carbon in first part
Potassium capacity method：Potassium bichromate and first part's sample are added in the sulfuric acid solution of a concentration of 1mol/L, sulfuric acid solution is heated to
It is 180 DEG C to maintain temperature, after the 5min that boils, stops heating, titrates containing for remaining potassium bichromate by ferrous sulfate again at this time
Amount, and then by the potassium bichromate of consumption, come in determination sample whether contain organic carbon.
When measuring containing organic carbon, then the first sample is placed at 800 DEG C -900 DEG C, is ashed 30min, removes the first sample
In the organic carbon that contains, place cooling.
The second part of second sample is for detecting whether contain sulfide mineral：Take second part and a concentration of 0.15mol/
The hydrochloric acid solution of L mixes, and is positioned over right over the container of the reaction using Lead acetate paper, since sulfide and hydrochloric acid meet
The hydrogen sulfide gas that will produce afterwards can leave brown spot when hydrogen sulfide encounters Lead acetate paper on Lead acetate paper, into
And can determine in sample whether contain sulfide.
When containing sulfide in determination sample, instilling 8 the first secondary solvents of drop makes the first sample all soak, and passes through the first pair
Solvent removes the sulfide mineral contained in the first sample, obtains pretreatment product at this time.
S3 is dissolved by heating
Pretreatment product are positioned in the conical flask of 25ml, main solvent 15ml is added, shake up and sample is made all to moisten.It again will cone
Shape bottle is placed on adjustable electric furnace, is heated rapidly to 245 DEG C -250 DEG C, while being stirred continuously with the glass bar with thermometer, is protected
15min is held, stirring fully obtains solidliquid mixture.
S4, cold filtration
After removing conical flask, be cooled to 40 DEG C -50 DEG C at room temperature, add 80 DEG C of distilled water 45ml, it is stirring while adding
It is even, after substance in conical flask is gone in beaker, be used in combination hot distilled water to rinse thermometer, glass bar and conical flask, and by washing lotion
It pours into beaker, distillation water inventory is added to be 200ml and stir evenly.Quantitative filter paper folding funnel at a slow speed is taken, leakage is positioned over
It is soaked in bucket and with distilled water.
Beaker is positioned on electric furnace, is heated to boiling, slightly stand, after suspended matter slightly settles, is filtered while hot, in filter paper
On obtain sediment.After filtering, beaker is cleaned with the hydrochloric acid of a concentration of 0.1mlol/L, and pickling is also carried out to sediment, is rushed
It washes 5 times, reusable heat distilled water cleans up the hydrochloric acid on sediment, until the pH of sediment is neutrality.
S5, after-treatment
The folded filter paper for having sediment is positioned on crucible for several times, dry on electric furnace, carbonize, capping and small there are one when charing
Seam, places into high-temperature electric resistance furnace, is ashed at 800 DEG C -900 DEG C, continues 30min.It takes out after the completion, is put into drying at room temperature
Cooling 1h in device, and write down the weight m of the substance obtained at this time1.The substance after ashing is positioned over platinum crucible after the completion of cooling
In, the second secondary solution is added, the addition sequence of the second secondary solution is the sulfuric acid solution that a concentration of 9mol/L of 5-8 drops is first added,
The sediment by ashing is all soaked, adds the hydrofluoric acid of 10ml a concentration of 40%, at this time the titanium dioxide in sediment
Silicon is fully dissolved in the second secondary solution.
Heating platinum crucible burns until not in white cigarette of emerging obtained substance to be placed in 900 DEG C of electric furnace at this time, this
When silica all evaporate, obtain waste residue, write down slag quality be m2。
S6 is weighed and is calculated
The weight of record necessary material is remembered in after-treatment and is passed through wherein the quality of the first sample is denoted as m in time during experiment
The material mass of ashing is m1, remember that the quality of waste residue is m2.The content of free silicon dioxide is w=(m in air known to then1-
m2)/m × 100%.
It is influenced to further reduce error, when above-mentioned experiment carries out, is additionally provided with one group of blank assay group.Blank test
The no test specimen of group, but the amount of reagent and step operated in above-mentioned experiment the first sample it is identical.Then it is ashed in S5
When, the quality m after the ashing of filter paper can be obtained3As corrected parameter, free silicon dioxide in revised air is obtained
Content is w=(m1-m2-m3)/m × 100%.
Particularly, in this programme although S1 and S2 is context in step, but in practical operation, can be synchronized
It carries out, can be that more people synchronize and carry out when conditions permit.Sample collection in S1 synchronous can be carried out with the measurement of impurity in S2,
Solvent preparation can prepare corresponding solvent, and the measurement of the organic carbon and sulfide mineral in S2 after the completion of impurity determination
Progress can be synchronized, the time of experiment will not be not only extended, once organic carbon or sulfide mineral are not contained in sample, so that it may with straight
Connect the operating time for shortening and removing and changing substance.
Embodiment 2：A kind of method of free silica content in detection air, difference lies in operations with embodiment 1
Technological parameter in step, specifically, during sample collection in S1, solvent are prepared, the sample of acquisition be placed in 108 DEG C of temperature into
Row is dried.By collected dust be directly divided into the first sample and the second sample totally two parts when, obtained the first sample matter
Amount is 0.2g.
Embodiment 3：A kind of method of free silica content in detection air, difference lies in operations with embodiment 1
Technological parameter in step, specifically, in the sample pretreatment of S2, ashing time is 35min when removing organic carbon.
Embodiment 4：A kind of method of free silica content in detection air, difference lies in operations with embodiment 1
Technological parameter in step is stirred specifically, distilled water is added in S4 and is 50 DEG C in conical flask, and final addition distillation
The total amount of water is 155ml.
Embodiment 5：A kind of method of free silica content in detection air, difference lies in operations with embodiment 1
Technological parameter in step, specifically, in the after-treatment of S5, the ashing duration to sediment is 35min；It is secondary to be added dropwise second
The hydrofluoric acid added when solution is 5ml.
Comparative example：According to GBZ/T192.4-2007《The 4th part of dust determination in workplace air：Free silicon dioxide
Content》Described in conversion the content of free silicon dioxide in air is measured.
Test portion
6 groups of experiments are carried out according to embodiment 1-5 and comparative example, measure the content of free silicon dioxide in the air of different zones,
And the duration of 6 groups of experiments is recorded, the human factor removed in operating process influences, and the when a length of standard consumed with comparative example
Experiment duration and the difference of standard duration that embodiment 1-5 is consumed are recorded into table 1 by duration.
The difference for the experiment duration and standard duration that 1 embodiment 1-5 of table is consumed
| Embodiment | Whether organic carbon is contained | Whether sulfide mineral is contained | Difference (min) |
| Embodiment 1 | Have | Have | -5 |
| Embodiment 2 | Have | Nothing | -14 |
| Embodiment 3 | Nothing | Nothing | -23 |
| Embodiment 4 | Have | Have | -3 |
| Embodiment 5 | Nothing | Have | -12 |
Data explanation
As shown in Table 1, the difference of the experiment duration consumed in embodiment 1-5 and standard duration is negative, therefore institute's used time
Between be shorter than standard duration, meanwhile, by embodiment 2,3 and 5 it can also be seen that, when detection substance do not contain organic carbon and/or vulcanization
When mineral, the time of shortening becomes apparent, likewise, removing the operation of corresponding impurity due to reducing, reduces to test sample
The impurity source of product also improves the precision of experiment to a certain extent.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of method of free silica content in detection air, which is characterized in that include the following steps：
S1, sample collection, solvent are prepared, and the solvent includes main solvent and secondary solvent, the coke that the main solvent is a concentration of 85%
Phosphoric acid solution, the pair solvent include at least the first secondary solvent of the ammonium nitrate solution of a concentration of 2mol/L, by a concentration of 9mol/
The sulfuric acid solution of L and a concentration of 40% hydrofluoric acid solution composition the second secondary solvent in one kind；
S2, sample pretreatment carry out the sample obtained in S1 to contain miscellaneous measurement：Organic carbon is carried out to the sample collected in S1
Assay, when sample detection when containing organic carbon, the sample collected in S1 is ashed at 800 DEG C -900 DEG C 30min-35min,
Sulfide mineral assay is carried out to the sample collected in S1, when sample detection Containing Sulfur mineral, instills described first
Secondary solvent removes sulfide mineral, obtains pretreatment product；
S3 is dissolved by heating, and product will be pre-processed described in S2 and the main solvent mixes, and be heated to 245 DEG C -250 DEG C, persistently stirred
15min is mixed, solidliquid mixture is obtained；
S4, cold filtration filter the solidliquid mixture in S3 with filter paper, obtain sediment, and weigh the quality of the sediment；
S5, after-treatment, by S4 filter paper and sediment be ashed 30min-35min at 800 DEG C -900 DEG C, be added described second
Secondary solvent, and continue heating until not emitting white cigarette, the calcination at 900 DEG C obtains waste residue；
S6 is weighed and is calculated, and completes the quality of weighing waste residue after after-treatment, free silicon dioxide in air is obtained by calculation
Content.
2. the method for free silica content in a kind of detection air according to claim 1, which is characterized in that by S1
Middle obtained sample of collecting separates 0.1g-0.2g as the first sample, remaining is the second sample, and first sample is for measuring two
The content of silica, second sample are used to carry out to contain miscellaneous measurement in the S2.
3. the method for free silica content in a kind of detection air according to claim 2, which is characterized in that work as institute
State the second sample detection when containing organic carbon, first sample is ashed at 800 DEG C -900 DEG C 30min-35min processing, when
When the second sample detection Containing Sulfur mineral, to instilling the described first secondary solvent in first sample, and by described first
Sample all soaks.
4. the method for free silica content in a kind of detection air according to claim 3, which is characterized in that described
The sample acquired in S1 is placed in 102 DEG C -108 DEG C of temperature and is dried, and drying time continues 2h, completes dry postcooling extremely
Room temperature, and sample is ground, until sample surfaces are smooth.
5. the method for free silica content in a kind of detection air according to claim 3, which is characterized in that described
When cooling in S4, temperature is down to 40 DEG C -50 DEG C, then by solidliquid mixture and 50 DEG C -80 DEG C of steaming that volume is 150ml-200ml
Distilled water is mixed evenly.
6. the method for free silica content in a kind of detection air according to claim 3, which is characterized in that described
Filter paper carries out pickling processes after sediment is obtained by filtration, first to the sediment, then washes spent pickling acid by distilled water, directly
Sediment is extremely washed till neutrality.
7. the method for free silica content in a kind of detection air according to claim 6, which is characterized in that described
When pickling processes, rinsed 3-5 times using the hydrochloric acid solution of a concentration of 0.1mol/L, and to sediment.
8. the method for free silica content in a kind of detection air according to claim 3, which is characterized in that described
When the second secondary solvent being added in S5, the sulfuric acid solution of a concentration of 9mol/L of 5-8 drops is first added, the sediment by ashing is complete
Portion soaks, and adds the hydrofluoric acid of 5ml-10ml a concentration of 40%.
9. the method for free silica content in a kind of detection air according to claim 3-8 any one, special
Sign is, when detecting free silica content in air, is provided with blank control group, the blank control group operating procedure with
The operating procedure of first sample is identical.
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| US11940376B2 (en) | 2022-03-29 | 2024-03-26 | Anhui University of Science and Technology | System and method for detecting concentration of free SiO2 in coal dust |
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