CN108106755A - calorimeter acceptance method - Google Patents
calorimeter acceptance method Download PDFInfo
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- CN108106755A CN108106755A CN201711289236.1A CN201711289236A CN108106755A CN 108106755 A CN108106755 A CN 108106755A CN 201711289236 A CN201711289236 A CN 201711289236A CN 108106755 A CN108106755 A CN 108106755A
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- calorimeter
- thermal capacity
- main phase
- acceptance
- acceptance method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K19/00—Testing or calibrating calorimeters
Abstract
The present invention relates to calorimeters to check and accept field, discloses a kind of calorimeter acceptance method, which includes：0.7 ± 0.055g, 1.3 ± 0.01g and (0.7g ± 0.055) g is respectively adopted, the thermal capacity of calorimeter and main phase Wen Sheng are measured by method of oxygen steel bomb with the standard substance benzoic acid of 4 incremental 0.097 0.13g values between (1.3 ± 0.01) g, if linear correlation between main phase Wen Shengyu thermal capacity, instrument is checked and accepted unqualified.Both it may determine that the problem of calorimeter whether there is equipment deficiency, the thermal capacity of a definite value can also be calibrated.The equipment of method acceptance(check) using the present invention fair and just can reliably detect data to providing true and accurate with coal unit and coal supply unit.
Description
Technical field
The present invention relates to calorimeter fields, and in particular to a kind of calorimeter acceptance method.
Background technology
Whether calorimeter thermal capacity is constant very big to the calorific value determination influences of coal, in same room temperature environment and sample matter
It,, then can not Accurate Determining such as still using fixed thermal capacity if thermal capacity rises and significant changes with inner cylinder temperature in the case that amount is certain
The calorific value of coal.So data, palpus are reliably detected to providing true and accurate with coal unit and coal supply unit to be fair and just
It holds calorimeter thermal capacity and checks and accepts pass.Existing calorimeter acceptance method includes：
(1) JJG 672-2001 People's Republic of China (PRC) national metrological verification regulations《Oxygen bomb calorimeter vertification regulation》In only
It provides the thermal capacity that combustion heat standard substance benzoic acid is used to examine and determine calorimeter 5 times, difference is defined by different mean heat capacities
It is very poor, then only respectively made once of the endpoints thereof of (0.7-1.3) g, it is average twice.This kind of acceptance method be can not check instrument and be asked
Topic.
(2)GB/T 213-2008《The heat output determining method of coal》, precision：The phase of 5 benzoic acid replication results
0.20% is not more than to standard deviation；Accuracy：The test result of certified reference coal and the difference of standard value are all in range of uncertainty
(lay particular emphasis on and how to carry out coal sample, science is a little)；Or by the use of benzoic acid as sample carry out 5 heating-value determinations, average value with
The difference of standard calorific value be no more than 50J/K, if be still with 1g it is invalid, equal to again demarcated a thermal capacity.Also it can not check instrument
Device problem.
(3)GB/T 213-2008《The heat output determining method of coal》10.9 clause concrete regulations determine its thermal capacity
The method of efficient working range, but do not elaborate for the intermediate range of (0.7-1.3) g.Instrument can be found
There is no problem also bad judgement.
Manufacturer does not require in client, carries out the debugging of equipment as stated above, so, it can not check instrument
The equipment deficiency that device is likely to cause in transport or assembling.
The content of the invention
The purpose of the invention is to overcome calorimeter acceptance method existing in the prior art can not check instrument transport or
The problem of equipment deficiency being likely to cause during assembling, provides a kind of calorimeter acceptance method.
To achieve these goals, the present invention provides a kind of calorimeter acceptance method, which is characterized in that the calorimeter is checked and accepted
Method includes：Be respectively adopted 0.7 ± 0.055g, 1.3 ± 0.01g and (0.7g ± 0.055) g between (1.3 ± 0.01) g with
The standard substance benzoic acid of 4 incremental 0.097-0.13g values measures the thermal capacity of calorimeter and main phase by method of oxygen steel bomb
Wen Sheng, if linear correlation between main phase Wen Shengyu thermal capacity, instrument is checked and accepted unqualified.
Calorimeter acceptance method using the present invention, directly by judging whether have substantially between main phase Wen Shengyu thermal capacity
Linear dependence, both may determine that the problem of calorimeter whether there is equipment deficiency, the heat of a definite value can also be calibrated
Capacity.The equipment of method acceptance(check) using the present invention can be fair and just to providing true standard with coal unit and coal supply unit
Really reliable detection data.
Specific embodiment
The endpoint of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For numberical range, between the endpoint value of each scope, respectively
It between the endpoint value of a scope and individual point value and can be individually combined with each other between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of calorimeter acceptance method, wherein, which includes：It is respectively adopted 0.7
± 0.055g, 1.3 ± 0.01g and (0.7g ± 0.055) g between (1.3 ± 0.01) g with 0.097-0.13g (for example,
0.1g, 0.11g, 0.12g, 0.13g) the standard substance benzoic acid of incremental 4 values pass through method of oxygen steel bomb and measure calorimeter
Thermal capacity and main phase Wen Sheng, if linear correlation between main phase Wen Shengyu thermal capacity, instrument is checked and accepted unqualified.
In the present invention, " linear dependence " refers to can be by the method for a linear equation or one-variable linear regression
The relational expression of the increasing or decreasing between main phase Wen Sheng and thermal capacity is acquired, i.e., according to tandem between main phase Wen Sheng and thermal capacity
It is increasing or less and less trend, in the linear dependence of predominate trend.
In the present invention, the concrete operations of the method for oxygen steel bomb may refer to GB/T 213-2008, the method for oxygen steel bomb
Basic principle：A certain amount of sample is burnt in the oxygen bomb filled with excessive oxygen, liberated heat is absorbed by certain water,
The caloric value of sample is calculated according to the rise of water temperature.To measure the caloric value of sample exactly according to above-mentioned principle, it is necessary to
It solves two problems, one is that the thermal capacity of instrument to be known in advance namely the Calorimetry system temperature of the instrument raise 1 DEG C of needs
The heat of absorption, this can be solved by using the primary standard substance benzoic acid calibrating instrument of known calorific value；Second be Calorimetry system with
Extraneous heat exchange problem, because the Calorimetry system of calorimeter is complicated, in addition to water absorbs heat, oxygen bomb, inner cylinder, thermometer
It can all absorb heat with blender etc., and respective heat absorption situation is different (specific heat capacity of a variety of materials is different), it is impossible to rely on
Simple numerical calculation obtains, and can only actually calibrate every liter of Calorimetry system temperature using the primary standard substance benzoic acid of known calorific value
The heat that is absorbed required for high 1 DEG C namely the thermal capacity for calibrating calorimeter.
In the present invention, if linear correlation between main phase Wen Shengyu thermal capacity, instrument examination is unqualified, if thermal capacity
Without apparent systematic change in the range of entire main phase temperature rises variation, i.e., without apparent linear dependence, then calorimetric
The thermal capacity of instrument can be considered as a constant, then instrument examination reaches a standard.
The calibration of thermal capacity is measured using the endpoints thereof of 0.7-1.3g in GB/T 213-2008, as the main phase Wen Shengyu of appearance
Thermal capacity will use the method for simple regression to acquire the relation of main phase Wen Shengyu thermal capacity, this kind of method there are during linear relationship
The relation of thermal capacity and main phase Wen Sheng can be solved, but laboratory personnel, when doing caloric value, each testing result cannot be direct
It uses, detection data will be recalculated by the unary linear regression equation derived, first, mistake is susceptible to, second is that sample
The task on the same day is not finished when more, also, this method can not detect instrument built-in problem.
The method of the present invention is compared with the thermal capacity calibration method in GB/T 213-2008, it can be ensured that directly calibrates
The definite value of one thermal capacity, meanwhile, it can find out more instrument problems, it is more rigorous to the examination of calorimeter.
In the present invention, when linear correlation between main phase Wen Shengyu thermal capacity, if over the increase heat of main phase Wen Sheng
Capacity is incremented by into apparent, then the caloric value that coal is made of the calorimeter will appear from gradually higher calorie value；If over master
The increase thermal capacity of phase Wen Sheng is into significantly successively decreasing, then the caloric value that coal is made of the calorimeter will appear from gradually relatively low heat
Value, reason can be found in the calculation formula of following formula caloric value：
QB, ad=[E* (tn-to+c)—(q1+q2)]/m
In formula：
QB, ad--- it is air-dried the heating quantity of bomb cylinder of sample, unit J/g；
The thermal capacity of E-calorimeter, unit J/k；
q1--- point is burning hot, unit J；
q2--- the total amount of heat of the additive such as generations such as bag paper, unit J；
M-sample mass, unit g；
C-cooling corrected value, unit are DEG C；
tnThe latter stage temperature of-inner cylinder, unit are DEG C；
t0The initial temperature of-inner cylinder, unit are DEG C.
tn-toFor main phase Wen Sheng, work as tn-toIt is big with 1 ton of coal 1 exemplified by measuring coal sample when there is apparent correlation with E
0.10 yuan of calculating of card, poor 100 kilocalorie is exactly 10.00 yuan, and such as burn 1,600,000 tons of coals, then is ten thousand yuan of 160*10=1600, thus may be used
To find out, main phase Wen Shengyu thermal capacity is all a considerable number to coal supply and with coal both sides there are linear dependence, is lost
Science fair.
In the present invention, under preferable case, (0.7g ± 0.055) g to 4 values between (1.3 ± 0.01) g is with 0.11-
0.12g is incremented by；Under most preferred case, (0.7g ± 0.055) g to 4 values between (1.3 ± 0.01) g is incremented by with 0.12g.
Under above-mentioned most preferred case, calorimeter can be more scrupulously checked and accepted.
It, can be according to the method in GB/T 213-2008, by 0.7 ± 0.055g and 1.3 ± 0.01g standards in the present invention
Substance benzoic acid replication 2 times.
The experiment condition and real material of the calorimeter acceptance method of the present invention will meet the requirement of GB/T213-2008.
For example, standard substance benzoic acid is the benzoic flake by dry and tabletting.Calorimetric substance on the basis of benzoic acid, it is second-class or second-class
More than, standard calorific value through authoritative metrological service determines or can clearly be traceable to authoritative metrological service.The benzoic acid is done
Dry condition can include：Dry 3 days or the dry 3-4h in 60-70 DEG C of baking oven in the drier for filling the concentrated sulfuric acid.Use note
Meaning item be：Sampling appliance answers clean dried, prevents from polluting；The acicular crystal on benzoic flake surface is brushed off using small, to prevent
Incomplete combustion.
The present invention will be described in detail by way of examples below.In following embodiment and comparative example, benzoic flake is
State Administration for Quality Supervision and Inspection and Quarantine ratifies, the city that the trade mark by China National Measuring Science Research Inst.'s production is GBW (E) 130035
Sell product, and 3 days dry, tabletting, with the small needle-shaped knot for brushing off benzoic flake surface in the drier for filling the concentrated sulfuric acid by it
It is brilliant.
Embodiment 1
Check and accept the calorimeter A that object is available from Sande Science and Technology Development Co., Ltd., Hunan model SDC311.According to GB/T
The main phase that automatic oxygen bomb calorimeter method measure in 213-2008 is detected according to the benzoic flake of the different quality shown in table 1
Wen Sheng and thermal capacity, the results are shown in Table 1.
Table 1
| Benzoic flake quality/g | Thermal capacity (J/K) | Inner cylinder initial stage temperature t0/℃ | Inner cylinder latter stage temperature tn/℃ | Main phase Wen Sheng/DEG C |
| 0.7230 | 5909.14 | 27.6023 | 30.9872 | 3.75 |
| 0.7345 | 5916.38 | 27.1297 | 30.6499 | 3.69 |
| 0.8432 | 5920.86 | 27.1062 | 31.1128 | 3.63 |
| 0.9410 | 5925.92 | 27.1777 | 31.6173 | 3.61 |
| 1.0469 | 5953.69 | 27.1665 | 32.0541 | 3.63 |
| 1.1583 | 5956.15 | 27.3684 | 32.7252 | 3.52 |
| 1.2999 | 5960.94 | 27.2591 | 30.7691 | 3.51 |
| 1.3001 | 5961.52 | 27.2075 | 33.3063 | 3.52 |
Come as can be seen from Table 1, thermal capacity and main phase Wen Sheng have apparent linear dependence, tentatively judge the calorimeter
It is subject to external impacts in transportational process, the temperature-sensing probe and AD cards of calorimeter inner cylinder may be damaged, and the resolution ratio of thermometric is low, AD
Card shows that reading is not allowed.The temperature-sensing probe of the calorimeter and AD cards are replaced, re-starts examination, the results are shown in Table 2.
Table 2
| Benzoic flake quality/g | Thermal capacity (J/K) | Inner cylinder initial stage temperature t0/℃ | Inner cylinder latter stage temperature tn/℃ | Main phase Wen Sheng/DEG C |
| 0.7576 | 5955.04 | 27.4607 | 30.8949 | 3.4342 |
| 0.7534 | 5945.15 | 26.7772 | 30.4208 | 3.6436 |
| 0.8783 | 5950.53 | 26.9692 | 31.1104 | 4.1412 |
| 0.9961 | 5941.97 | 26.9269 | 31.6001 | 4.6732 |
| 1.0996 | 5954.80 | 27.2209 | 32.3396 | 5.1187 |
| 1.2099 | 5955.40 | 27.4061 | 33.0056 | 5.5995 |
| 1.3047 | 5956.94 | 27.5556 | 33.5661 | 6.0105 |
| 1.3050 | 5951.55 | 27.4817 | 33.4972 | 6.0155 |
As can be seen from Table 2, when carrying out an acceptance inspection again to the calorimeter for having replaced temperature-sensing probe and AD cards, thermal capacity and master
Phase Wen Sheng does not have linear dependence, also, the very poor of the thermal capacity measured is 25.85J/K, and relative standard deviation 0.1%, exists
In national standard (GB/T 213-2008) allowed band, then the examination of the calorimeter after component is replaced and has reached a standard.The present embodiment is said
Bright, acceptance method using the present invention can not only check and accept thermal capacity, can also check and accept out calorimeter with the presence or absence of instrument problems.
Comparative example 1
Object is checked and accepted with embodiment 1, before carrying out an acceptance inspection to it according to the method for embodiment 1, first by it according to GB/T
Automatic oxygen bomb calorimeter method in 213-2008 measure according to shown in table 3 different quality ((0.7g ± 0.055) g to (1.3 ±
0.01) value between g is incremented by with 0.05-0.07g) the main phase Wen Sheng that detects of benzoic flake and thermal capacity, as a result such as table 3
It is shown.
Table 3
Thermal capacity and main phase Wen Shengcheng non-linear dependencies it can be seen from the result of table 3, there is no check and accept out instrument to ask
Topic.
For same calorimeter, (0.7g ± 0.055) g it can be seen from the results contrast of embodiment 1 and comparative example 1
When being incremented by the value between (1.3 ± 0.01) g with 0.05-0.07g, thermal capacity and main phase Wen Shengcheng non-linear dependencies, not
Detect instrument problems；And (0.7g ± 0.055) g to the value between (1.3 ± 0.01) g be with 0.097-0.13g it is incremental 4
During a value, the thermal capacity and the main phase temperature that detect rise linear correlation, detected the instrument that comparative example 1 does not detect and ask
Topic.Therefore, calorimeter acceptance method of the invention can more scrupulously check and accept calorimeter.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In the skill of the present invention
In art conception range, a variety of simple variants can be carried out to technical scheme, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, belongs to
Protection scope of the present invention.
Claims (5)
1. a kind of calorimeter acceptance method, which is characterized in that the calorimeter acceptance method includes：Be respectively adopted 0.7 ± 0.055g,
1.3 ± 0.01g and (0.7g ± 0.055) g between (1.3 ± 0.01) g with the standards of incremental 4 values of 0.097-0.13g
Substance benzoic acid measures the thermal capacity of calorimeter and main phase Wen Sheng by method of oxygen steel bomb, if having between main phase Wen Shengyu thermal capacity
Linear dependence, then instrument examination is unqualified.
2. calorimeter acceptance method according to claim 1, wherein, (0.7g ± 0.055) g is between (1.3 ± 0.01) g
4 values be incremented by with 0.11-0.12g.
3. calorimeter acceptance method according to claim 2, wherein, (0.7g ± 0.055) g is between (1.3 ± 0.01) g
4 values be incremented by with 0.12g.
4. the calorimeter acceptance method according to any one in claim 1-3, wherein, by 0.7 ± 0.055g and 1.3 ±
0.01g standard substance benzoic acid replication 2 times.
5. the calorimeter acceptance method according to any one in claim 1-3, wherein, standard substance benzoic acid is process
Dry and tabletting benzoic flake.
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| CN201711289236.1A CN108106755A (en) | 2017-12-07 | 2017-12-07 | calorimeter acceptance method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1376911A (en) * | 2001-03-27 | 2002-10-30 | 湘潭工学院 | Analysis linearizing and automatic heat capacity compensating method for intelligent calorimeter |
| CN1381720A (en) * | 2002-04-26 | 2002-11-27 | 长沙三德实业有限公司 | Calorimeter for measuring temp of sandwich |
| CN1388371A (en) * | 2002-07-19 | 2003-01-01 | 长沙三德实业有限公司 | Electrothermally-calibrated calorimetric instrument |
| US20060045164A1 (en) * | 2004-08-31 | 2006-03-02 | Schuh William C | System and method of compensation for device mounting and thermal transfer error |
| CN105606649A (en) * | 2016-03-09 | 2016-05-25 | 西安近代化学研究所 | High-activity aluminum powder combustion heat measurement method |
-
2017
- 2017-12-07 CN CN201711289236.1A patent/CN108106755A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1376911A (en) * | 2001-03-27 | 2002-10-30 | 湘潭工学院 | Analysis linearizing and automatic heat capacity compensating method for intelligent calorimeter |
| CN1381720A (en) * | 2002-04-26 | 2002-11-27 | 长沙三德实业有限公司 | Calorimeter for measuring temp of sandwich |
| CN1388371A (en) * | 2002-07-19 | 2003-01-01 | 长沙三德实业有限公司 | Electrothermally-calibrated calorimetric instrument |
| US20060045164A1 (en) * | 2004-08-31 | 2006-03-02 | Schuh William C | System and method of compensation for device mounting and thermal transfer error |
| CN105606649A (en) * | 2016-03-09 | 2016-05-25 | 西安近代化学研究所 | High-activity aluminum powder combustion heat measurement method |
Non-Patent Citations (1)
| Title |
|---|
| 米娟层: "谈谈热量计的验收方法", 《煤质技术》 * |
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