CN101799388A - Method and apparatus for measuring gas forming quantity of calcium carbide by using single calibrating weight method - Google Patents

Method and apparatus for measuring gas forming quantity of calcium carbide by using single calibrating weight method Download PDF

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CN101799388A
CN101799388A CN201010112143A CN201010112143A CN101799388A CN 101799388 A CN101799388 A CN 101799388A CN 201010112143 A CN201010112143 A CN 201010112143A CN 201010112143 A CN201010112143 A CN 201010112143A CN 101799388 A CN101799388 A CN 101799388A
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gas
carbide
calcium
forming amount
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周振华
史玉奎
周晨旭
李凤超
周俐君
张成东
周勇
王楠楠
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周振华
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Abstract

The invention relates to a method and an apparatus for measuring the gas forming quantity of calcium carbide by using a single calibrating weight method, belonging to the technical field of chemical detection. The apparatus for measuring the gas forming quantity of calcium carbide by using a single calibrating weight method comprises a weight weighing machine, a reactor and a gas purifier, wherein a gas inlet of the gas purifier is connected with a gas outlet of the reactor; the reactor and the gas purifier are arranged on the upper part of the weight weighing machine; and the weight weighing machine weighs the weight of the reactor and the gas purifier. In addition, the invention also provides a method for detecting the gas forming quantity of the calcium carbide by utilizing mass variation values before and after the weighed calcium carbide reacts with water. The invention has accurate measurement data, simple and convenient operation method, small volume of the measurement device, low price, convenient use and verification and convenient generalization and popularization.

Description

Single calibration weight method is surveyed the method and the apparatus of carbide of calcium gas forming amount
Technical field
The present invention relates to a kind of single calibration weight method and survey the method and the apparatus of carbide of calcium gas forming amount, belong to the chemical detection technique field.
Background technology
The production of present domestic carbide of calcium, trade, applying unit are substantially all lack of standardization to the mensuration of gas forming amount, even the quality of quality is just judged by some entity and individual by the severe degree of visual inspection carbide of calcium and water reaction, the reason that causes above this situation is that traditional measurement method is according to the size of how much judging the carbide of calcium gas forming amount that produces the acetylene gas volume, because the measurement gas volume is subjected to extraneous multiple condition effect easily, so this measuring method has significant limitation.
According to the regulation of " carbide of calcium (calcium carbide) " standard GB 10665-2004, the gas forming amount that carbide of calcium dispatches from the factory is at 260-350L/Kg; To require sample size 50g to calculate in the GB, under standard state, splendid attire gas containers volume must not be less than 17.5L (regulation be the gasometer of 19L in the GB), so equipment price costliness of existing survey carbide of calcium gas forming amount, bulky, can't carry, and that its maximum shortcoming is a checking procedure is very loaded down with trivial details, complicated, measurement result is subjected to external environment influence such as temperature, air pressure very big, standard, gasometer etc. need irregular verification, and the verification condition is very strict, deals with inspection so equipment is only bought by some producer, unactual use.Therefore, the method mensuration carbide of calcium gas forming amount of a kind of simple possible of research exploration has important practical significance to effective comprehensive utilization of carbide of calcium.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, provide a kind of determination data accurate, method of operating is simple, convenient, and the determinator volume is small and exquisite, cheap, the use verification is convenient, and single calibration weight method of being convenient to popularize is surveyed the method and the apparatus of carbide of calcium gas forming amount.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of single calibration weight method is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that, comprises weight scales, reactor and gas purifier; The air intake opening of gas purifier links to each other with the gas outlet of reactor, and reactor and gas purifier are located at the top of weight scales, the weight of weight scales weighing reactor and gas purifier.
Described reactor is that volume is not less than the 250ml container.Preferably, reactor is that volume is the 500-2000ml bottle,suction.
Described weight scales is the balance that precision is not less than 0.2 gram.Preferably, weigher is precision 0.1 a gram electronic balance.
Described gas purifier comprises except that water-bound, dedusting structure and water structure, the air intake opening that removes water-bound is connected with the gas outlet of reactor, the gas outlet of removing water-bound is connected with the air intake opening of dedusting structure by one section drying tube that is filled with water absorbing agent, and the water filling port of water structure is connected with the air intake opening that removes water-bound.Preferably, remove water-bound and be condenser pipe, more excellent, removing water-bound is spiral cold-finger.Preferably, dedusting structure is the strip tubular structure, is filled with absorbent cotton in the pipe.Preferably, water structure is the glass tube that has cock, the water inlet of water structure with remove water-bound and be connected, the water delivering orifice of water structure is connected with draft tube except that water-bound.
The gas outlet of above-mentioned dedusting structure also is connected with the check structure, and the gas outlet of dedusting structure links to each other with the air intake of check structure, and the gas outlet of check structure communicates with atmosphere.Preferably, described check structure is the U-shaped tubulose, fills water absorbing agent in the pipe.
Preferably, water absorbing agent is an anhydrous calcium chloride.
A kind of single calibration weight method is surveyed the method for carbide of calcium gas forming amount, it is characterized in that, the mass change value of utilizing weighing carbide of calcium and water to react front and back is come the gas forming amount of detection computations carbide of calcium, and concrete steps are as follows:
(1) weight of weighing carbide of calcium sample, reaction water and surveying instrument device, addition obtains reacting preceding general assembly (TW);
(2) carbide of calcium is mixed with reaction water until reacting completely;
(3) weight of residual reaction afterproduct in reacted surveying instrument device of weighing and the surveying instrument device, addition obtains reacting the back general assembly (TW);
(4) deduct reaction back general assembly (TW) with general assembly (TW) before the reaction and obtain difference DELTA m, and calculate gas forming amount according to difference DELTA m, formula is as follows:
Figure GSA00000047274700021
G is the gas forming amount of sample in the formula, the L/Kg of unit; V AcetyleneBe the volume of acetylene gas, the m of unit 3Δ m unit is Kg; T is a kelvin degree under the standard state, unit K; R is a gas law constant 8.314, and the J/ of unit (mol * K); P is an atmospheric pressure under the standard state, the Pa of unit; m Carbide of calciumBe the sample quality of weighing, unit K g; M AcetyleneBe acetylene molecule quality, unit K g/mol.
Described reaction water is the aqueous solution of the saturated mistake of acetylene.The aqueous solution of the saturated mistake of acetylene i.e. this aqueous solution again can't dissolved acetylene gas, and the preparation method is this area conventional method.
This detection side's ratio juris is as follows:
The reaction of carbide of calcium and reaction water generates acetylene gas, and produce with a large amount of water vapours and dust this moment, utilizes dedusting and removes water-bound and separate and discharge acetylene gas; By the changing value of quality before and after the surveying instrument device internal reaction thing, calculate the quality of acetylene gas
CaC 2+2H 2O→C 2H 2↑+Ca(OH) 2
Can draw according to gas equation PV=nRT that (20 ℃, the volume V of gas in the time of 101.3Kpa), the ratio of acetylene gas volume and carbide of calcium sample weighting amount are exactly gas forming amount G (L/Kg) in standard state.
Calculation sample standard state (20 ℃ during gas forming amount in the time of 101.3Kpa), are utilized the defined formula of gas forming amount:
According to reaction equation and equation for ideal gases, can calculate:
Figure GSA00000047274700023
Thereby can calculate the gas forming amount of carbide of calcium
Figure GSA00000047274700024
G is the gas forming amount of sample in the formula, the L/Kg of unit; V AcetyleneBe the volume of acetylene gas, the m of unit 3Δ m unit is Kg; T is a kelvin degree under the standard state, unit K; R is a gas law constant 8.314, and the J/ of unit (mol * K); P is an atmospheric pressure under the standard state, the Pa of unit; m Carbide of calciumBe the sample quality of weighing, unit K g; M AcetyleneBe acetylene molecule quality, unit K g/mol.
The assay method of above carbide of calcium gas forming amount, sample granularity is 5-12mm during sampling, and sort out obvious visible silicon-iron block in the sample, it should be noted that the sample surfaces powdered substance removes totally as far as possible, these powdered substances are a part of carbide of calcium and the reacted product of airborne water, and the mensuration of gas forming amount is had certain influence.
Beneficial effect of the present invention:
(1) the present invention carries out the detection of carbide of calcium gas forming amount by the quality of measuring acetylene gas, because the quality of gas is compared with volume, is not subject to the influence of external environment, numerical stability, and can directly calculate standard state (20 ℃, the gas forming amount of carbide of calcium sample in the time of 101.3Kpa); Therefore than classic method, verification of the present invention is simple, accuracy is high, easy and simple to handle.
(2) because pick-up unit has saved the gasometer of measuring gas volume, reduce the volume and weight of pick-up unit greatly, made pick-up unit be convenient for carrying.
(3) owing to needn't collect the gas of generation in the testing process, therefore can significantly improve sample weighting amount, reduce the influence of accidentalia, thereby improve method precision and accuracy, make testing result more near the value of getting angry of actual detected product to testing result.Through experiment, utilize this method or apparatus to measure the not restriction of examined example weight in theory, usually the sample result of one-time detection 30-300g is comparatively desirable, and general sample weighting amount is 100 grams, and only is 50g according to the value of traditional national standard method one-time detection sample.
(4) because the verification of Weight-measuring device verification relative and volume measurement device is convenient, so the present invention will be significantly less than the verification maintenance cost of conventional detection devices to the verification maintenance cost of checkout equipment.
(5) condensate water that utilizes condensation to remove water-bound can be used as the reaction water of carbide of calcium sample simultaneously, thereby makes device compact, small and exquisite more; Weight scales can portablely be used simultaneously, so package unit can be carried convenient the use.
(6) precision is the electronic balance of 0.1 gram, and measuring accuracy can reach 1.85L/Kg, is better than the 4L/Kg of GB, and can be by strengthening sample weighting amount or selecting for use more high-precision weight scales further to improve the method precision.
Description of drawings
Fig. 1 is the structural representation that the single calibration weight method of the present invention is surveyed carbide of calcium gas forming amount apparatus;
Wherein: 1, weight scales, 2, reactor, 3, gas purifier, 4, water structure, 5, spiral cold-finger, 6, drying tube, 7, dedusting structure, 8, the check structure, 9, anhydrous calcium chloride.
Embodiment
The present invention will be further described below in conjunction with drawings and Examples, but institute of the present invention protection domain is not limited thereto.
Embodiment
A kind of single calibration weight method is surveyed the apparatus of carbide of calcium gas forming amount, as shown in Figure 1, comprises weight scales 1, reactor 2 and gas purifier 3; The air intake opening of gas purifier 3 links to each other with the gas outlet of reactor 2, and reactor 2 and gas purifier 3 are located at the top of weight scales 1, the weight of weight scales 1 weighing reactor 2 and gas purifier 3.Described reactor 2 is the bottle,suction of volume 1000ml.Described weight scales 1 is the electronic balance of precision 0.1 gram.Described gas purifier 3 comprises spiral cold-finger 5, dedusting structure 7 and water structure 4, the air intake opening of spiral cold-finger 5 is connected with the gas outlet of reactor 2, and the gas outlet of spiral cold-finger 5 is connected with the air intake opening of dedusting structure 7 by one section drying tube 6 that is filled with anhydrous calcium chloride 9.Described dedusting structure 7 is the strip tubular structure, is filled with absorbent cotton in the pipe.Described water structure 4 is for having the glass tube of cock, and the water inlet of water structure 4 is connected with spiral cold-finger 5 bottoms, and the water delivering orifice of water structure 4 is connected with the draft tube of spiral cold-finger 5.The gas outlet of dedusting structure 7 also is connected with check structure 8, and this check structure 8 is the U-shaped tubulose, fills anhydrous calcium chloride 9 in the pipe.
The condensation mode of dewatering is more suitable for detection of the present invention and numerical evaluation, and the gas-liquid separation effect of spiral cold-finger is better than straight tube condenser pipe and spherical condensation tube.
The check structure is the water removal effect that is used to detect except that water-bound, improves the accuracy of apparatus testing result.
Utilize apparatus of the present invention and method contrast " carbide of calcium " GB 10665-2004 standard to further specify accuracy of the present invention below.
Following test apparatus device is the described apparatus of present embodiment, sampling, method for making sample by requirement among " carbide of calcium " GB 10665-2004, produce gas forming amount each 500g of carbide of calcium about 300L/Kg and 280L/Kg, compare test with method and the apparatus stipulated among the method that the present invention relates to and apparatus and " carbide of calcium " GB 10665-2004 behind the sample mixing, test procedure is as follows, and test findings sees Table 1:
1, the water of the saturated mistake of preparation acetylene, the calibrated electronic balance;
2, the water of filling medicine, the saturated mistake of acetylene connects the determining instrument device;
3, claim carbide of calcium sample 100g, be accurate to 0.1g, be designated as m Carbide of calcium
4, sample is put into dry good reactor, with calibrated electronic balance reactor, gas purifier integral body is weighed, and is designated as m 1
5, add the water of acetylene saturated mistake by water structure to reactor by gas purifier, drip speed and drip/second for 1-3;
6, along with the carrying out of reaction, progressively strengthen inflow, open fully up to cock;
7, after liquid level maintains an equal level, close the water structure cock, once more reactor, gas purifier are weighed, be designated as m 2
8, each parameter bring into formula basis of calculation state (20 ℃, 101.3Kpa) the carbide of calcium gas forming amount G (L/Kg) under
Figure GSA00000047274700042
Figure GSA00000047274700043
Table 1
National standard method, is measured according to " carbide of calcium " GB 10665-2004 predetermined operation simultaneously by full-time technician in the table 1.Approaching by above contrast test measurement result of the present invention as can be seen and National Standard Method measurement result numerical value, can substitute detection fully.

Claims (10)

1. the apparatus of a single calibration weight method survey carbide of calcium gas forming amount is characterized in that, comprises weight scales, reactor and gas purifier; The air intake opening of gas purifier links to each other with the gas outlet of reactor, and reactor and gas purifier are located at the top of weight scales, the weight of weight scales weighing reactor and gas purifier.
2. single calibration weight method as claimed in claim 1 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that described reactor is that volume is not less than the 250ml container; Preferably, reactor is that volume is the 500-2000ml bottle,suction.
3. single calibration weight method as claimed in claim 1 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that, described weight scales is the balance that precision is not less than 0.2 gram; Preferably, weigher is precision 0.1 a gram electronic balance.
4. single calibration weight method as claimed in claim 1 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that, described gas purifier comprises except that water-bound, dedusting structure and water structure, the air intake opening that removes water-bound is connected with the gas outlet of reactor, the gas outlet of removing water-bound is connected with the air intake opening of dedusting structure by one section drying tube that is filled with water absorbing agent, and the water filling port of water structure is connected with the air intake opening that removes water-bound.
5. single calibration weight method as claimed in claim 4 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that, removes water-bound and is condenser pipe, and more excellent, removing water-bound is spiral cold-finger.
6. single calibration weight method as claimed in claim 4 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that dedusting structure is the strip tubular structure, is filled with absorbent cotton in the pipe.
7. single calibration weight method as claimed in claim 4 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that, water structure is the glass tube that has cock, the water inlet of water structure with remove water-bound and be connected, the water delivering orifice of water structure is connected with draft tube except that water-bound.
8. single calibration weight method as claimed in claim 4 is surveyed the apparatus of carbide of calcium gas forming amount, it is characterized in that the gas outlet of above-mentioned dedusting structure also is connected with the check structure; Preferably, described check structure is the U-shaped tubulose, fills water absorbing agent in the pipe; Preferably, water absorbing agent is an anhydrous calcium chloride.
9. the method for a single calibration weight method survey carbide of calcium gas forming amount is characterized in that the mass change value of utilizing weighing carbide of calcium and water to react front and back is come the gas forming amount of detection computations carbide of calcium, and concrete steps are as follows:
(1) weight of weighing carbide of calcium sample, reaction water and surveying instrument device, addition obtains reacting preceding general assembly (TW);
(2) carbide of calcium is mixed with reaction water until reacting completely;
(3) weight of residual reaction afterproduct in reacted surveying instrument device of weighing and the surveying instrument device, addition obtains reacting the back general assembly (TW);
(4) deduct reaction back general assembly (TW) with general assembly (TW) before the reaction and obtain difference DELTA m, and calculate gas forming amount according to difference DELTA m, formula is as follows:
Figure FSA00000047274600011
G is the gas forming amount of sample in the formula, the L/Kg of unit; V AcetyleneBe the volume of acetylene gas, the m of unit 3Δ m unit is Kg; T is a kelvin degree under the standard state, unit K; R is a gas law constant 8.314, the J/mol * K of unit; P is an atmospheric pressure under the standard state, the Pa of unit; m Carbide of calciumBe the sample quality of weighing, unit K g; M AcetyleneBe acetylene molecule quality, unit K g/mol.
10. single calibration weight method as claimed in claim 9 is surveyed the method for carbide of calcium gas forming amount, it is characterized in that described reaction water is the aqueous solution of the saturated mistake of acetylene.
CN2010101121433A 2010-02-23 2010-02-23 Method and apparatus for measuring gas forming quantity of calcium carbide by using single calibrating weight method Expired - Fee Related CN101799388B (en)

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CN108844869A (en) * 2018-06-06 2018-11-20 山西省环境科学研究院 A kind of flue dust on-line sampling and weighing device and method
CN109900588A (en) * 2019-03-20 2019-06-18 国家镁及镁合金产品质量监督检验中心 Activated carbon content detection device and detection method in a kind of novel magnesium powder
CN110508218A (en) * 2019-08-16 2019-11-29 中国地质科学院水文地质环境地质研究所 The measurement method of Zero-valent Iron hydrodynamic seepage pressure hydrogen producing amount and precipitation capacity
CN111398091A (en) * 2020-03-05 2020-07-10 柳州钢铁股份有限公司 Analysis method for determining calcium carbide in composite silicon carbide deoxidizer for steelmaking

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CN102928056A (en) * 2012-11-22 2013-02-13 中国人民解放军国防科学技术大学 Method for measuring coking quantity of hydrocarbon fuel
CN102928056B (en) * 2012-11-22 2016-01-06 中国人民解放军国防科学技术大学 The measuring method of hydrocarbon fuel coking amount
CN108844869A (en) * 2018-06-06 2018-11-20 山西省环境科学研究院 A kind of flue dust on-line sampling and weighing device and method
CN108844869B (en) * 2018-06-06 2024-04-12 山西省生态环境监测和应急保障中心(山西省生态环境科学研究院) Online smoke dust sampling and weighing device and method
CN109900588A (en) * 2019-03-20 2019-06-18 国家镁及镁合金产品质量监督检验中心 Activated carbon content detection device and detection method in a kind of novel magnesium powder
CN110508218A (en) * 2019-08-16 2019-11-29 中国地质科学院水文地质环境地质研究所 The measurement method of Zero-valent Iron hydrodynamic seepage pressure hydrogen producing amount and precipitation capacity
CN111398091A (en) * 2020-03-05 2020-07-10 柳州钢铁股份有限公司 Analysis method for determining calcium carbide in composite silicon carbide deoxidizer for steelmaking

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