CN109668876A - The apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability - Google Patents
The apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability Download PDFInfo
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- CN109668876A CN109668876A CN201710964764.6A CN201710964764A CN109668876A CN 109668876 A CN109668876 A CN 109668876A CN 201710964764 A CN201710964764 A CN 201710964764A CN 109668876 A CN109668876 A CN 109668876A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The present invention relates to the apparatus for quantitatively and purposes of a kind of industrial nitrocelluloses long-term chemical durability, mainly solve the problems, such as in the prior art can only qualitative test and nitrous tolerance can not be quantitative determined.The present invention by using a kind of industrial nitrocelluloses long-term chemical durability apparatus for quantitatively, including testing tube, metal bath, drier, oven, buret, testing tube includes the glass tube of lower part and the condenser on top, it is connected by ground, at least one testing tube is placed in metal bath, oven is used for the predrying of test specimen, drier is used to carry out re-dry to the test specimen after predrying, buret, which is used to be in control experimentation middle and lower part glass liquid, carries out alkali-titration, the nitrous gas flow released by measuring every gram of nitrocellulose, whether judgement sample there is the technical solution of long-term chemical durability preferably to solve the above problem, it can be used in the quantitative test of industrial nitrocelluloses long-term chemical durability.
Description
Technical field
The present invention relates to a kind of apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability.
Background technique
The stabilization processes of industrial nitrocelluloses are a steps conclusive, crucial in nitrocellulose production process,
For obtain in entire storage period it is dangerous without spontaneous combustion, can transport safely and use, stable industrial nitrocelluloses product, must
Stabilization processes and suitable control must be carried out to each production batch.Therefore, to judge industrial nitrocelluloses stabilization processes
It whether is able to satisfy transport, storage, requirement afterwards, it is necessary to carry out the long-term chemical durability test of nitrocellulose.With me
State standardizes hazardous chemical management increasingly, and various means of testing are gradually perfect, and the present invention is in hazardous chemical working unit, respectively
There is comparable application and popularization value in kind chemical company.It is domestic that test side not yet is provided to industrial nitrocelluloses chemical stability
Method, to the change under industrial nitrocelluloses high temperature in external " dangerous cargo international road transports European Convention " (2015 editions ADR)
Although learning stability test has respective specified, but a kind of qualitative test method, the judgment criteria of stability are not stringent enough.
The present invention and the chemical stability under " dangerous cargo international road transports European Convention " (2015 editions ADR) high temperature
Whether test method is different, judge whether nitrocellulose has the method for chemical stability in ADR, generated in observation experiment
Nitrous gas is a kind of qualitative test method, cannot quantitative determine the amount of the nitrous gas of generation, and is tested used in the present invention
Test device in device and ADR is also different.
Summary of the invention
The first technical problem to be solved by the present invention be in the prior art can only qualitative test and Asia can not be quantitative determined
The problem of niter air amount, provides a kind of apparatus for quantitatively of new industrial nitrocelluloses long-term chemical durability, and having can be fixed
The advantages of nitrous tolerance is determined in measurement.The second technical problem to be solved by the present invention be to provide it is a kind of with the technical issues of solution it
The purposes of the apparatus for quantitatively of one corresponding industrial nitrocelluloses long-term chemical durability.
One of in order to solve the above problem, The technical solution adopted by the invention is as follows: a kind of industrial nitrocelluloses long life
The apparatus for quantitatively of stability is learned, including testing tube, metal bath, drier, oven, buret, testing tube include lower part
The condenser of container and top, is connected by ground, at least one testing tube is placed in metal bath, and oven is used for test specimen
Predrying, drier be used for after predrying test specimen carry out re-dry, buret be used for experimentation middle and lower part
Container obtains liquid and carries out alkali-titration, the nitrous gas flow released by measuring every gram of nitrocellulose, and judgement sample is
It is no that there is long-term chemical durability.
In above-mentioned technical proposal, it is preferable that carry out industrial nitrocelluloses long-term chemical durability using described device
Quantitative test includes the following steps:
(1) it before testing, first has to that nitrocellulose is dried;
(2) it after predrying, by nitrocellulose sample by being ground up, sieved or cutting into pieces, is placed on containing melting
Or in the vacuum desiccator of granular calcium chloride, dry 15h or more;For the nitrocellulose of weak nitrification, using containing dense sulphur
The drier of acid is dried, drying time at least 15h.
(3) test sample is put into testing tube, testing tube bottom container and condenser is assembled;
(4) according to the difference of testing tube condenser shape, water is poured into the ball room of condenser, and ensures that no water enters
Into testing tube bottom container;
(5) after the temperature of constant-temperature metal bath reaches set temperature, each testing tube is inserted into the aperture of constant temperature bath, is surveyed
The depth that test tube is submerged is 110-220mm, records the time that experiment starts;
(6) in experimentation, unless observed smoke event, otherwise testing tube temperature maintains experimental temperature;If
It observes and smolders, stop test immediately, and record heating time;
(7) testing tube is after the time that experimental temperature heating is subscribed, by cooling, cooling procedure after testing tube removal constant temperature bath
In, a part of water can flow into the container of lower part;After cooling, the liquid in condenser is moved on in bottom container;
(8) liquid in bottom container is moved on in another container, at this point, 175mL is not to be exceeded in total amount of liquid;
(9) it is titrated, is judged by calculating, if the nitrous gas that 1g nitrocellulose releases with sodium hydroxide solution
Less than 2.5mL, then it is assumed that it is with long-term chemical stability.
In above-mentioned technical proposal, it is preferable that before experiment, first have to that nitrocellulose is dried;According to be increase
The nitrocellulose for moulding nitrocellulose and weak nitrification, carry out predrying before the drying, predrying in ventilated oven into
Row, is heated, until the quality of mitigation in every 15 minutes is less than the 0.3% of proper mass.
In above-mentioned technical proposal, it is preferable that vacuum desiccator pressure should be in 6.5kPa or less.
In above-mentioned technical proposal, it is preferable that the nitrocellulose moisture content after dry is lower than 1%.
In above-mentioned technical proposal, it is preferable that the frosted regions of thorough rubbing test pipe bottom container and condenser assembling,
Silica gel is uniformly smeared at frosted regions, then assembles container and condenser.
In above-mentioned technical proposal, it is preferable that if protecting screen has been used in experiment, when testing tube is put into or removes constant temperature bath
When, it is necessary to the open side of careful rotation protecting screen is against wall or the depletion region in room;If without protecting screen, using anti-
Face shield protection face.
In above-mentioned technical proposal, it is preferable that calculation method:
In formula, VNOFor the volume of the NO of generation, cm3/g;cNaOHFor the concentration of caustic soda, 0.01mol/L;VNaOHFor consumption
The volume of caustic soda, mL;VNO,mFor the molal volume of NO, 22.38L/mol;mNCFor the quality of nitrocellulose, g.
In above-mentioned technical proposal, it is preferable that be made into indicator using 1% alcohol and 8g methyl red and 3g crystal violet, use
The sodium hydroxide solution of 0.01mol/L is titrated.
In order to solve the above problem two, The technical solution adopted by the invention is as follows: a kind of industrial nitrocelluloses long life
Learn the purposes of the apparatus for quantitatively of stability, the quantitative test for industrial nitrocelluloses long-term chemical durability.
The present invention designs stability in use testing tube and carries out the experiment of nitrocellulose chemical stability, by the nitrification of 1 or 2g
Cellulose sample is put into stability test pipe, heating 2h is carried out in 132 DEG C ± 1 DEG C of constant-temperature metal bath, with the side of alkalimetric titration
Method measures the amount of the nitrous gas of heating process release, if the nitrous gas that 1g nitrocellulose releases is less than 2.5mL, then it is assumed that
It is with long-term chemical stability.Compared with chemical stability test under nitrocellulose high temperature in ADR, the present invention passes through steady
Qualitative test pipe collects the nitrous gas generated, and later-stage utilization alkalimetric titration method calculates the amount of the nitrous gas of generation, by fixed
Amount method judges the long-term chemical durability of nitrocellulose, and Rule of judgment is more stringent, and the conclusion of acquisition is more reliable, obtains
Preferable technical effect.
Detailed description of the invention
Fig. 1 is nitrocellulose stability test pipe structure chart.
In Fig. 1, left side is the glass tube of testing tube lower part, and right side is the condenser on testing tube top.1 --- grinding port plug,
2 --- condenser ball room top ground, 3 --- condenser ball room, 4 --- condenser ball room, 5 --- grinding port plug, 6 --- glass
The ground of pipe, 7 --- glass tube.When experiment, nitrocellulose sample is added in the glass tube in left side, top connection condensation
Device.Grinding port plug 1 is connect with ground 2 in figure, and grinding port plug 5 is connect with ground 6, and the assembling of stability test pipe can be completed.
Fig. 2 is experiment schematic diagram.
In Fig. 2,1 --- metal bath;2 --- it is packed into the stability test pipe after sample.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[embodiment 1]
A kind of apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability, nitrocellulose stability test pipe
As shown in Figure 1, left side is the glass tube of testing tube lower part in Fig. 1, right side is the condenser on testing tube top.When experiment, by nitre
Cellulose sample is added in the glass tube in left side, and top connects condenser.Grinding port plug 1 is connect with ground 2 in figure, grinding port plug 5
It is connect with ground 6, the assembling of stability test pipe can be completed.
The quantitative stability that the present invention is suitable for various types nitrocellulose is tested.
1, test philosophy:
1 or 2g nitrocellulose sample is put into stable pipe, is heated two hours in 132 DEG C of ± 1 DEG C of constant-temperature metal baths,
The amount that the nitrous gas of heating process release is measured with the method for alkalimetric titration, if the nitrous gas that 1g nitrocellulose releases is less than
2.5mL, then it is assumed that it is with long-term chemical stability.
2, test equipment:
(1) the stability test pipe that designs of the present invention: testing tube lower part be length be 270-330mm, internal diameter is about
The transparent glass tube that 17.5mm, outer diameter are about 19.5mm, combined number of the top condenser to match.
(2) precision is 10mg or the higher assay balance of precision.
(3) vacuum desiccator, the drier containing the super concentrated sulfuric acid containing melting or granular calcium chloride.
(4) ventilated oven.
(5) constant-temperature metal bath: Wood's metal metal bath uses the thermometer or thermocouple (precision is 0.1 DEG C) prison of calibration
Survey bath temperature.
(6) polycarbonate protective screen or safety cabinet.
(7) the semi-automatic pipette of 10mL.
(8) the wide neck conical flask of 250mL.
(9) testing tube of 50mL.
(10) buret of 10-25mL.
(11) glass funnel.
3, agents useful for same is tested:
(1) sodium hydroxide solution.
(2) pH indicator: such as methyl orange acid, methyl red, methyl red/methylenum careuleum or R8, B3 color indicator
(Tacchiro).The solution that alcohol and 8g methyl red and 3g crystal violet in this test using 1% mix.
(3) fully deionized water or distilled water of the conductivity less than 1 μ S.
4, testing procedure:
(1) it before testing, first has to that nitrocellulose is dried.According to be plasticising nitrocellulose and weak nitrification
Nitrocellulose, to carry out predrying before the drying.Predrying carries out in ventilated oven.Oven temperatures are set as 70
DEG C, it is heated, until the quality of mitigation in every 15 minutes is less than the 0.3% of proper mass.
(2) it after predrying, at room temperature, by nitrocellulose sample by being ground up, sieved or cutting into pieces, puts
It sets in the vacuum desiccator containing melting or granular calcium chloride, is paved into very thin one layer, dry 15h or more.In drier
Pressure should be in 6.5kPa or less.It for the nitrocellulose of weak nitrification, is dried, is done using the drier containing the super concentrated sulfuric acid
At least 15h of dry time.
(3) 1g or 2g drying nitrocellulose (moisture content has to be lower than 1%) is weighed using assay balance, is accurate to 1mg
(weigh 3g and be plasticized nitrocellulose, be accurate to 1mg).Sample is put into dry and clean testing tube using funnel, thoroughly
The frosted regions of rubbing test pipe bottom glass pipe and condenser assembling, can uniformly smear silica gel, then at frosted regions
Glass tube and condenser are assembled.
(4) according to the difference of testing tube condenser shape, the distilled water of 15-50mL is weighed, is poured into the ball room of condenser.
Simultaneously, it is ensured that no water enters in testing tube bottom glass pipe.
(5) when confirming that the temperature of constant-temperature metal bath reaches 132 DEG C ± 1 DEG C, each testing tube is inserted into the hole of constant temperature bath
In mouthful.Different according to the shape of constant temperature bath, the depth that test tube is submerged is different, but submergence must be in 110mm to 220mm
Between, the time that experiment starts is recorded at this time.
If protecting screen has been used in experiment, when testing tube is put into or removes constant temperature bath, it is necessary to careful rotation protection
The open side of screen is against wall or the depletion region in room.If should be protected using protective face mask without protecting screen
Mask portion.
(6) in experimentation, unless observed the phenomenon that smoldering, otherwise testing tube temperature maintains 132 DEG C ± 1 DEG C two
A hour.If it is observed that smoldering, then stopping test immediately, and heating time is recorded.
After heating two hours (plasticising nitrocellulose heats a hour) at (7) 132 DEG C, testing tube is removed into constant temperature
Bath, and be placed on bracket, it is cooled down after protecting screen.In this period, a part of water can be flowed into the glass tube of lower part.
After 30 minutes cooling, the liquid in condenser is moved on in bottom glass pipe, with distilled water flushing condenser.
(8) liquid in bottom glass pipe is moved on in conical flask, and cleans testing tube with distilled water.At this point, liquid is total
175mL is not to be exceeded in amount.
(9) it is titrated with sodium hydroxide solution.
5, calculation method:
In formula, VNOFor the volume of the NO of generation, cm3/g;cNaOHFor the concentration of caustic soda, 0.01mol/L;VNaOHFor consumption
The volume of caustic soda, mL;VNO,mFor the molal volume of NO, 22.38L/mol;mNCFor the quality of nitrocellulose, g.
Judged by calculating, if the nitrous gas that 1g nitrocellulose releases is less than 2.5mL, then it is assumed that it has long-term
Chemical stability.
With reference to the accompanying drawing and specific embodiment the invention will be further described.
(1) certain industry nitration cotton being subjected to predrying, is put into ventilated oven, set temperature is 70 DEG C, it is heated, until
Until the quality mitigated for every 15 minutes is less than the 0.3% of proper mass.
(2) after predrying, at 20 DEG C, which is cut into pieces, be placed on containing melting or
In the vacuum desiccator of granular calcium chloride, it is paved into very thin one layer, dry 15h.
(3) transparent glass tube on the left of 3 Fig. 1 of distilled water flushing is used, and is dried with instrument drying box, with assay balance point
The dry nitrocellulose sample of 1g is weighed three times, is accurate to 0.001g.Sample is respectively put into 3 transparent glass tubes by funnel
In, ground D and grinding port plug C in Fig. 1 is thoroughly wiped, and uniformly smear silica gel, then condenses right side in glass tube and 3 Fig. 1
Device assembling.
(4) distilled water for weighing 50mL respectively, is poured into the ball room of 3 condensers.
(5) temperature of constant-temperature metal bath is set as 132 DEG C, 3 testing tubes are inserted into the aperture of constant temperature bath, and insertion is deep
150mm is spent, time started, two hours of heated at constant temperature are recorded.
(6) testing tube is removed into constant temperature bath, and be placed on bracket, cooled down after protecting screen.After 30 minutes cooling,
With distilled water flushing condenser.
(7) liquid in bottom glass pipe is moved on in conical flask, and cleans glass tube with distilled water.
(8) indicator is made into using 1% alcohol and 8g methyl red and 3g crystal violet, be added in conical flask, used
The sodium hydroxide solution of 0.01mol/L is titrated.
(9) with the formula calculate 3 testing tubes in nitrocellulose generate nitrous gas be respectively 2.332mL,
2.31mL and 2.354mL, therefore judge that the industrial nitrocelluloses are the products with long-term chemical durability.
[comparative example]
Below with reference to comparative example, invention is further explained, test philosophy, instrument, reagent, step, calculation method
It is all the same with preceding embodiment 1, specific implementation step is described below:
(1) certain industry nitration cotton B is subjected to predrying, is put into ventilated oven, set temperature is 70 DEG C, is heated, directly
Until the quality that every 15 minutes mitigate is less than the 0.3% of proper mass.
(2) after predrying, at 20 DEG C, which is cut into pieces, be placed on containing melting or
In the vacuum desiccator of granular calcium chloride, it is paved into very thin one layer, dry 15h.
(3) transparent glass tube on the left of 3 attached drawings of distilled water flushing is used, and is dried with instrument drying box, assay balance is used
The dry nitrocellulose sample of 1g is weighed in three times, is accurate to 0.001g.Sample is respectively put into 3 transparent glass by funnel
Guan Zhong thoroughly wipes ground 6 and grinding port plug 5 in attached drawing, and uniformly smears silica gel, then by right side in glass tube and 3 attached drawings
Condenser assembling.
(4) distilled water for weighing 50mL respectively, is poured into the ball room of 3 condensers.
(5) temperature of constant-temperature metal bath is set as 132 DEG C, 3 testing tubes are inserted into the aperture of constant temperature bath, and insertion is deep
150mm is spent, time started, two hours of heated at constant temperature are recorded.
(6) testing tube is removed into constant temperature bath, and be placed on bracket, cooled down after protecting screen.After 30 minutes cooling,
With distilled water flushing condenser.
(7) liquid in bottom glass pipe is moved on in conical flask, and cleans glass tube with distilled water.
(8) indicator is made into using 1% alcohol and 8g methyl red and 3g crystal violet, be added in conical flask, used
The sodium hydroxide solution of 0.01mol/L is titrated.
(9) with the formula calculate 3 testing tubes in nitrocellulose generate nitrous gas be respectively 2.761mL,
2.794mL and 2.75mL, the amount of the nitrous gas of three groups of Self -adaptives judge the industrial nitrocelluloses more than 2.5mL
It is the product without long-term chemical durability.
Claims (10)
1. a kind of apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability, including testing tube, metal bath, drying
Device, oven, buret, testing tube include the container of lower part and the condenser on top, are connected by ground, at least one testing tube
It is placed in metal bath, oven is used for the predrying of test specimen, and drier is used to carry out again the test specimen after predrying
Dry, buret is used to obtain experimentation middle and lower part container liquid to carry out alkali-titration, by measuring every gram of nitrocellulose
Whether the nitrous gas flow that element releases, judgement sample have long-term chemical durability.
2. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 1, it is characterised in that
The quantitative test that industrial nitrocelluloses long-term chemical durability is carried out using described device, is included the following steps:
(1) it before testing, first has to that nitrocellulose is dried;
(2) after predrying, by nitrocellulose sample by being ground up, sieved or cut into pieces, be placed on containing melt or
In the vacuum desiccator of granular calcium chloride, dry at least 15h;For the nitrocellulose of weak nitrification, using containing the concentrated sulfuric acid
Drier is dried, drying time at least 15h.
(3) test sample is put into testing tube, testing tube bottom container and condenser is assembled;
(4) according to the difference of testing tube condenser shape, water is poured into the ball room of condenser, and ensures that no water enters survey
In test tube bottom container;
(5) after the temperature of constant-temperature metal bath reaches set temperature, each testing tube is inserted into the aperture of constant temperature bath, testing tube
The depth being submerged is 110-220mm, records the time that experiment starts;
(6) in experimentation, unless observed smoke event, otherwise testing tube temperature maintains experimental temperature;If observation
To smoldering, stop test immediately, and record heating time;
(7) testing tube, will be cooling after testing tube removal constant temperature bath after the time that experimental temperature heating is subscribed, in cooling procedure,
A part of water can flow into the container of lower part;After cooling, the liquid in condenser is moved on in bottom container;
(8) liquid in bottom container is moved on in another container, at this point, 175mL is not to be exceeded in total amount of liquid;
(9) it is titrated, is judged by calculating, if the nitrous gas that 1g nitrocellulose releases is less than with sodium hydroxide solution
2.5mL, then it is assumed that it is with long-term chemical stability.
3. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
Before experiment, first have to that nitrocellulose is dried;According to be plasticized nitrocellulose and weak nitrification nitrocellulose
Element will carry out predrying before the drying, and predrying is carried out in ventilated oven, heated, and mitigate until every 15 minutes
Until quality is less than the 0.3% of proper mass.
4. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
Vacuum desiccator pressure should be in 6.5kPa or less.
5. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
Nitrocellulose moisture content after drying is lower than 1%.
6. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
The frosted regions of thorough rubbing test pipe bottom container and condenser assembling, uniformly smear silica gel at frosted regions, then will
Container and condenser assemble.
7. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
If protecting screen has been used in experiment, when testing tube is put into or removes constant temperature bath, it is necessary to the open side of careful rotation protecting screen
Depletion region facing to wall or room;If protecting face using protective face mask without protecting screen.
8. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
Calculation method:
In formula, VNOFor the volume of the NO of generation, cm3/g;cNaOHFor the concentration of caustic soda, 0.01mol/L;VNaOHFor the caustic soda of consumption
Volume, mL;VNO,mFor the molal volume of NO, 22.38L/mol;mNCFor the quality of nitrocellulose, g.
9. the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability according to claim 2, it is characterised in that
Indicator is made into using 1% alcohol and 8g methyl red and 3g crystal violet, is dripped with the sodium hydroxide solution of 0.01mol/L
It is fixed.
10. a kind of purposes of the apparatus for quantitatively of industrial nitrocelluloses long-term chemical durability is used for industry nitration fiber
The quantitative test of plain long-term chemical durability.
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Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105784701A (en) * | 2016-03-09 | 2016-07-20 | 西安近代化学研究所 | Testing system of nitrogen content of nitrocotton and detecting method of nitrogen content |
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CN105784701A (en) * | 2016-03-09 | 2016-07-20 | 西安近代化学研究所 | Testing system of nitrogen content of nitrocotton and detecting method of nitrogen content |
Non-Patent Citations (2)
Title |
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中国纤维素行业协会: "关于工业硝化棉产品安定性测试方法的函(附件1:贝克曼•荣克安定性测试方法)", 《WWW.CHINACIA.COM.CN/NEWS-SHOW-1537.ASPX》 * |
工业化学品: "交通运输部就《危险货物道路运输规则》行业标准(征求意见稿)公开征求意见(附件2:《危险货物道路运输规则 第2部分:分类》征求意见稿及编制说明)", 《HTTPS://WWW.REACH24H.COM/CHEMICAL/NEWS-CENTER/OTHER-REGULATION/1230-MOT-CONSULTS-ON-THE-PROVISIONS-OF-ROAD-TRANSPORT-OF-DANGEROUS-GOODS.HTML》 * |
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