CN108225968A - The assay method of urea content in a kind of NOx reducing agent aqueous solution of urea - Google Patents
The assay method of urea content in a kind of NOx reducing agent aqueous solution of urea Download PDFInfo
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- CN108225968A CN108225968A CN201711446467.9A CN201711446467A CN108225968A CN 108225968 A CN108225968 A CN 108225968A CN 201711446467 A CN201711446467 A CN 201711446467A CN 108225968 A CN108225968 A CN 108225968A
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- urea
- aqueous solution
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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
Abstract
The invention discloses a kind of assay methods of urea content in NOx reducing agent aqueous solution of urea, belong to technical field of quality detection.Technical problem solved by the invention is to provide the new method that a kind of easy to operate, of low cost, result accurately measures urea for vehicle content.The assay method of urea content, includes the following steps in a kind of NOx reducing agent aqueous solution of urea:NOx reducing agent aqueous solution of urea is placed in measuring cup, drying to constant weight, by weigh the cap upper grinding port plug, it is put into drier and is cooled to 15~25 DEG C, it weighs, deducts the mass fraction of biuret in aqueous solution of urea, you can calculate the content of urea in aqueous solution of urea.The method of the present invention can accurately measure the content of urea in urea for vehicle, and testing result favorable reproducibility, precision are high, and avoid the expensive instrument of purchase and using expensive raw material, greatly reduce testing cost, easy to operate, application easy to spread.
Description
Technical field
The invention belongs to technical field of quality detection, and in particular to urea in a kind of NOx reducing agent aqueous solution of urea
The assay method of content.
Background technology
Motor vehicle emission standard regulation, automotive emissions HC (hydrocarbon), NOx(nitrogen oxygenate),
CO (carbon monoxide), PM (particle) etc. are needed by the active layer of applied catalysis converter, air injection reaction and with cold
But the technologies such as exhaust gas recycling system of device, control and reduction automotive emissions could be discharged to specified value.Therefore
Selective catalytic reduction system operating is mounted in diesel engine exhaust system, by injecting NOx reducing agent-urea water
Oxynitrides in exhaust is catalysed and reduced into nitrogen and water, discharging pollutants for automobile can be made to reach emission request by solution.
It can be seen that the pressure with the standard is carried out, the usage amount of NOx reducing agent-aqueous solution of urea is more and more extensive, because
This, the content of urea is to ensure the important prerequisite of urea for vehicle quality in Accurate Determining solution.National regulation urea for vehicle quality
It is required that for 31.8~33.2%.
At present in GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea》In, AUS32 urea contains
Measure (total nitrogen method) method of amount, needs to establish standard curve, cumbersome, need to use combustion method nitrogen auto analyzer, the instrument
It is worth about 500,000 RMB, it is also necessary to which, using expensive high purity oxygen gas, nitrogen standard substance, cost is too high, economically
Consider, it is necessary instead of combustion method measure urea for vehicle content to establish new assay method.
Invention content
Technical problem solved by the invention be to provide a kind of easy to operate, of low cost, result accurately measure it is automobile-used
The method of urea content.
There is provided a kind of NOx reducing agent urea for technological means used by the present invention solves above-mentioned technical problem
The assay method of urea content, this method include the following steps in aqueous solution:
It is m that the NOx reducing agent aqueous solution of urea that quality is m is placed in quality0Band grinding port plug measuring cup in, institute
It states band grinding port plug measuring cup to be oven-dried in advance to constant weight, the band grinding port plug measuring cup of aqueous solution of urea will be filled in temperature 65~90
Drying to constant weight at DEG C, and measuring cup is uncapped drying in drying course, immediately by weigh the cap upper grinding port plug, is put into cold in drier
It to 15~25 DEG C, weighs, the gross mass for obtaining measuring cup is m1, the mass fraction of urea in aqueous solution of urea is calculated as follows:
In formula:ωUreaRepresent the mass fraction of urea in NOx reducing agent aqueous solution of urea;ωBiuretRepresent nitrogen oxidation
The mass fraction of biuret in object reducing agent aqueous solution of urea;M is 0.9000~5.1000g.
Wherein, it is described in NOx reducing agent aqueous solution of urea described above in the assay method of urea content
ωUreaIt is 31.8~33.2%.
Wherein, it is described in NOx reducing agent aqueous solution of urea described above in the assay method of urea content
ωBiuretNo more than 0.3%.
Wherein, it is described in NOx reducing agent aqueous solution of urea described above in the assay method of urea content
ωBiuretAccording to GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea (AUS 32)》Side in appendix C
Method measures to obtain.
Wherein, in NOx reducing agent aqueous solution of urea described above in the assay method of urea content, the nitrogen
The addition of oxide reducing agent aqueous solution of urea is 0.9000~5.1000g;The temperature of the drying is 65~90 DEG C;It is described
The time of drying is 1~8h.
Preferably, it is described in NOx reducing agent aqueous solution of urea described above in the assay method of urea content
The addition of aqueous solution of urea is 0.9000~1.1000g;The temperature of the drying is 65~75 DEG C;The time of the drying is
1~3h.
It is furthermore preferred that in NOx reducing agent aqueous solution of urea described above in the assay method of urea content, institute
The temperature for stating drying is 70 DEG C;The time of the drying is 2h.
Wherein, in NOx reducing agent aqueous solution of urea described above in the assay method of urea content, the baking
It does to the standard of constant weight and is:Sample is repeated to drying, cooling, weighing at the same temperature, until measure twice Xiang Cha≤
0.1%.
Wherein, in NOx reducing agent aqueous solution of urea described above in the assay method of urea content, the band
Grinding port plug measuring cup is diameter 40mm, high 25mm, and carries the glass measuring cup of strict grinding port plug.
Beneficial effects of the present invention:
The method of the present invention can accurately measure the content of urea in urea for vehicle, and testing result favorable reproducibility, precision are high,
With trackability, and the problem of buying expensive instrument and using expensive raw material is avoided, greatly reduce and measure automobile-used urine
The cost of cellulose content;The method of the present invention need not establish standard curve, easy to operate, and combustion method can be replaced to measure urea for vehicle and contained
Amount, application easy to spread.
Specific embodiment
Specifically, in a kind of NOx reducing agent aqueous solution of urea urea content assay method, this method include with
Lower step:
It is m that the NOx reducing agent aqueous solution of urea that quality is m is placed in quality0Band grinding port plug measuring cup in, institute
It states band grinding port plug measuring cup to be oven-dried in advance to constant weight, the band grinding port plug measuring cup of aqueous solution of urea will be filled in temperature 65~90
Drying to constant weight at DEG C, and measuring cup is uncapped drying in drying course, immediately by weigh the cap upper grinding port plug, is put into cold in drier
It to 15~25 DEG C, weighs, the gross mass for obtaining measuring cup is m1, the mass fraction of urea in aqueous solution of urea is calculated as follows:
In formula:ωUreaRepresent the mass fraction of urea in NOx reducing agent aqueous solution of urea;ωBiuretRepresent nitrogen oxidation
The mass fraction of biuret in object reducing agent aqueous solution of urea;M is 0.9000~5.1000g.
In the method for the present invention, the gross mass m of measuring cup1By the quality group of sample after measuring cup (including grinding port plug), drying
Into, and comprising urea and minute quantity biuret in sample after drying, therefore also need to deduct the content of biuret, it could be accurate
Obtain NOx reducing agent aqueous solution of urea in urea mass fraction.
The mass fraction of urea is 31.8~33.2% in current automobile-used NOx reducing agent-aqueous solution of urea, this hair
Bright method can efficiently, accurately measure its urea content.
ω in the method for the present inventionBiuretAccording to GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea
(AUS32)》Method in appendix C measures to obtain, and this method is:In the alkaline solution of sodium potassium tartrate tetrahydrate, biuret and divalent
Copper reaction generates a kind of aubergine compound, which has maximum absorption band at wavelength 550nm;With spectrophotometer in wave
The absorbance of the aubergine compound is measured at long 550nmm;Standard curve is depicted as, then by urea with biuret standard solution
The absorbance of aqueous sample calculates the concentration of biuret on standard curve.Automobile-used NOx reducing agent-aqueous solution of urea
The mass fraction of middle biuret is no more than 0.3%.
Weight, drying temperature and drying time are urinated by many experiments according in urea for vehicle used by the method for the present invention
The co-determinations such as the chemical property and energy conservation and environmental protection condition of element.Due to the urea in NOx reducing agent-aqueous solution of urea
The organic compound being made of carbon, nitrogen, oxygen and hydrogen, also known as urea, chemical formula CON2H4、(NH2)2CO or CN2H4O, fusing point
It is 132.7 DEG C.Using the property, optimum weight, drying temperature and drying time are found, obtains both accurately detecting in solution and urinate
Plain percentage composition, and the purpose for being thermally decomposed it.
By a large amount of screenings of the inventor to determination condition, in the method for the present invention, the addition of the aqueous solution of urea is
0.9000~5.1000g;The temperature of the drying is 65~90 DEG C;The time of the drying is 1~8h, in such measurement strip
Under part, it is ensured that the accuracy of result of the test avoids sample from not drying.
In order to ensure the accuracy of experimental result, consider with reference to the decomposition temperature of power consumption, urea, ensure that urea is not in solution
It is affected by temperature and decomposes, so as to fulfill testing result stabilization, can trace, precision is high.Preferably, the aqueous solution of urea
Addition is 0.9000~1.1000g;The temperature of the drying is 65~75 DEG C;The time of the drying is 1~3h;More preferably
, the temperature of the drying is 70 DEG C;The time of the drying is 2h.
The method of the present invention needs to dry aqueous solution of urea, therefore during drying, can make by grinding port plug tiltedly as on measuring cup
Measuring cup opens wide lid in drying course;Measuring cup generally selects diameter 40mm, high 25mm, and the glass with strict grinding port plug
Measuring cup;In order to ensure the accuracy of testing result, before adding in aqueous solution of urea, need that perseverance will be dried to grinding port plug measuring cup
Weight.
The standard that drying to constant weight in the method for the present invention is:Sample is repeated to drying, cooling, title at the same temperature
Amount until measuring Xiang Cha≤0.1% twice, ensures the accuracy of testing result;If more than this numerical value, then the sample is represented also
Drying, the urea content that thus numerical computations go out completely, including further including the moisture do not dried.
It is generally dried in air -oven in the method for the present invention, after drying to constant weight, will be ground in weigh the cap immediately
Mouthful plug, is put into drier and is cooled to room temperature, and so as to which moisture in air be avoided to influence the accuracy of result, room temperature is generally 15~
25℃。
The present invention is described in further detail below by test example and experimental example, but is not therefore protected the present invention
Scope limitation is among the embodiment described range.
It is accurate to prepare NOx reducing agent-aqueous solution of urea 1Kg that mass fraction is 32.15%, it is tested in the present invention
Example and experimental example use this solution.
Test example 1:The selection of drying temperature
1.0000g aqueous solution of urea is weighed, is put into the band grinding port plug measuring cup that drying to constant weight, by grinding port plug tiltedly extremely
In on measuring cup, the measuring cup equipped with sample is dried at 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C and 105 DEG C respectively
2h immediately by weigh the cap upper grinding port plug, is put into drier and is cooled to room temperature, weigh;According to GB 29518-2013《Diesel oil is sent out
Motivation NOx reducing agent aqueous solution of urea (AUS 32)》Method in appendix C measures ωBiuret;It the results are shown in Table 1.
Gained urea content (%) is measured under 1 different temperatures of table
Drying temperature | 65℃ | 70℃ | 75℃ | 80℃ | 85℃ | 90℃ | 105℃ |
Urea content | 32.17 | 32.16 | 32.16 | 32.04 | 31.91 | 31.85 | 31.30 |
As can be seen from Table 1, with the raising of temperature, the phenomenon that percentage composition of urea declines in solution, this is
There is decomposing phenomenon in urea during due to more than 80 DEG C in solution, and percentage composition continuously decreases, and 85 DEG C of whens reduce by 0.75%, 90 DEG C
When reduce by 0.94%, to 105 DEG C when then reduces by 2.64%, and error reaches 0.85, significantly larger than GB 29518-2013《Diesel oil
Engine NOx reducing agent aqueous solution of urea》The precision requirement of middle appendix A method.Therefore, in order to ensure experimental result
Accuracy, which dries aqueous solution of urea using 70 ± 5 DEG C, it is ensured that in solution urea be not affected by temperature and
It decomposes, so as to fulfill testing result stabilization, can trace, precision is high.
Test example 2:Drying time determines
Weigh 1.0000g urea liquids, be put into the band grinding port plug measuring cup that drying to constant weight, by grinding port plug tiltedly as
On measuring cup, the measuring cup equipped with sample at 65 DEG C, 70 DEG C, 75 DEG C is dried to 1h, 1.5h, 2h, 3h respectively, will be weighed immediately
Bottle cap upper grinding port plug, is put into drier and is cooled to room temperature, weigh;According to GB 29518-2013《Diesel engine nitrogen oxides is also
Former agent aqueous solution of urea (AUS 32)》Method in appendix C measures ωBiuret;It the results are shown in Table 2.
2 different time of table, at a temperature of measure gained urea content (%)
As shown in Table 2, at 65 DEG C, after drying 1 hour, urea content 100.31% is after drying 1.5 hours
100.16%, it after 100.06%, 3 hours is 100.00% that drying 2, which was as a child,;At 70 DEG C, after drying 1 hour, urea content
It is 100.22%, drying was 100.06% after 1.5 hours, was 100.00% after being 100.00%, 3 hours after drying 2 hours;
At 75 DEG C, after drying 1 hour, urea content 100.16%, drying was 100.16% after 1.5 hours, and drying is after 2 hours
It is 100.00% after 100.00%, 3 hours;Consider that it is 70 DEG C to select temperature with reference to the decomposition temperature of power consumption, urea, the time is
2h both ensure that the time more than needed, improves the accuracy of experiment, also saves power consumption.Thus the experiment uses and dries 2 at 70 DEG C
Hour, it is entirely capable of meeting test requirements document.Simultaneously for the accuracy of guarantee test result, sample is avoided not dry, then by sample
It is put into air -oven and dries, cools down repeatedly at similary temperature, weighing, be less than until measuring weight amount difference twice
0.0003g。
Test example 3:Example weight determines
It is representative in order to ensure to weigh sample, weigh respectively 1.0000g, 2.0000g, 3.0000g, 4.0000g and
5.0000g urea liquids are put into the band grinding port plug measuring cup that drying to constant weight, by grinding port plug tiltedly as on measuring cup, are incited somebody to action
Measuring cup equipped with sample dries 2h at 70 DEG C respectively, immediately by weigh the cap upper grinding port plug, is put into drier and is cooled to room
Temperature is weighed;According to GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea (AUS 32)》In appendix C
Method measure ωBiuret;It the results are shown in Table 3.
3 different quality sample of table dries urea content (%) obtained by 2h at 70 DEG C
As can be seen from Table 3, weigh different weight urea for vehicle dry 2h at 70 DEG C after, quality be 1g sample contain
Amount is stablized.Thus the experiment dries 2 hours at 70 DEG C using 1g samples are weighed, is entirely capable of meeting test requirements document.
Experimental example 1:Precision Experiment
6 groups of 1.0000g urea liquids are weighed, are put into the band grinding port plug measuring cup that drying to constant weight, grinding port plug is oblique
As on measuring cup, the measuring cup equipped with sample at 70 DEG C is dried into 2h respectively, immediately by weigh the cap upper grinding port plug, is put into
It is cooled to room temperature in drier, weighs;According to GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea
(AUS32)》Method in appendix C measures ωBiuret;It the results are shown in Table 4.
4 repeated experiment result of table
As shown in Table 4, the content for determining urea in urea for vehicle according to the new method, standard deviation 0.03%, thus
It can be seen that this method favorable reproducibility, has preferable precision.
Experimental example 2:The rate of recovery is tested
6 1.0000g urea for vehicle solution examples are weighed, are put into the band grinding port plug measuring cup that drying to constant weight, it will
Grinding port plug tiltedly as on measuring cup, is separately added into 0.0500g, 0.1000g, 0.1500g, 0.2000g, 0.2400g and 0.3000g
Measuring cup equipped with sample is dried 2h by urea at 70 DEG C respectively, immediately by weigh the cap upper grinding port plug, is put into drier
It is cooled to room temperature, carries out recovery of standard addition experiment.Result of the test is shown in Table 5.
5 rate of recovery experimental result of table
Add in urea amount/g | Recycle urea amount/g | The urea rate of recovery/% | |
1 | 0.0535 | 0.0536 | 100.19 |
2 | 0.1035 | 0.1028 | 99.32 |
3 | 0.1530 | 0.1524 | 99.61 |
4 | 0.2024 | 0.2009 | 99.26 |
5 | 0.2482 | 0.2484 | 100.08 |
6 | 0.3047 | 0.3030 | 99.44 |
By table 5 as it can be seen that sample for different urea contents, recovery of standard addition is 100 ± 1%, and therefore, new method is surveyed
The content accuracy for determining urea in urea for vehicle is high.By using new method, the content of urea in urea for vehicle can be accurately measured,
It solves the problems, such as to need to buy expensive instrument and using expensive raw material, and experimental result accuracy is high, has trackability.
Claims (9)
1. the assay method of urea content in NOx reducing agent aqueous solution of urea, it is characterised in that:Include the following steps:
It is m that the NOx reducing agent aqueous solution of urea that quality is m is placed in quality0Band grinding port plug measuring cup in, band mill
Mouthful plug measuring cup is oven-dried in advance to constant weight, and the band grinding port plug measuring cup for filling aqueous solution of urea is dried at 65~90 DEG C of temperature
It does to constant weight, measuring cup is uncapped drying in drying course, is immediately put into weigh the cap upper grinding port plug cold in drier after drying
It to 15~25 DEG C, weighs, the gross mass for obtaining measuring cup is m1, the mass fraction of urea in aqueous solution of urea is calculated as follows:
In formula:ωUreaRepresent the mass fraction of urea in NOx reducing agent aqueous solution of urea;ωBiuretRepresent nitrogen oxides also
The mass fraction of biuret in former agent aqueous solution of urea;M is 0.9000~5.1000g.
2. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 1
It is:The ωUreaIt is 31.8~33.2%.
3. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 1
It is:The ωBiuretNo more than 0.3%.
4. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 3
It is:The ωBiuretAccording to GB 29518-2013《Diesel engine NOx reducing agent aqueous solution of urea》In appendix C
Method measures to obtain.
5. according to the measure side of urea content in Claims 1 to 4 any one of them NOx reducing agent aqueous solution of urea
Method, it is characterised in that:The time of the drying is 1~8h.
6. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 5
It is:The addition of the NOx reducing agent aqueous solution of urea is 0.9000~1.1000g;The temperature of the drying is 65
~75 DEG C;The time of the drying is 1~3h.
7. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 5
It is:The addition of the NOx reducing agent aqueous solution of urea is 1.0000g;The temperature of the drying is 70 DEG C;It is described
The time of drying is 2h.
8. the assay method of urea content, feature in NOx reducing agent aqueous solution of urea according to claim 1
It is:The standard that drying to constant weight is that sample is put into air -oven and dries, cool down repeatedly at similary temperature, claiming
Amount, until measuring Xiang Cha≤0.1% twice.
9. according to the measure side of urea content in claim 1~8 any one of them NOx reducing agent aqueous solution of urea
Method, it is characterised in that:The band grinding port plug measuring cup is diameter 40mm, high 25mm, and the glass with strict grinding port plug claims
Measuring bottle.
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