Some standard content:
Verification Regulation for Oxygen Bomb Calorimeter
J.JG6722001
Verification Regulation for Oxygen Bomb Calorimeter
Verifkcation Regulation for the Homb Celorireler
J.IG 672-
Replaces I[G;672—
JCA73---(X:
The calibration standard has been approved by the State Quality Supervision and Inspection Administration in 2007 and was issued on January 1, 2001 Starting point:
Responsible unit: National Technical Committee for Chemical Metrology of China Drafting unit: Standard Dynamics Research Center This regulation is interpreted by the National Technical Qualifications of the State Council. The main drafter of this regulation:
Shu Xiuhui (National Standard Material Research Center) Participating drafter:
Chemical Sensitization (National Standard Material Research Center) [S0
Performance requirements
3. Price release
3.2 Salt content and blood density change-
3. Factors and tea
3.4 Total mass point stability...
Technical requirements
1.1 Appearance requirements of the net plate
4.2 Internal and external safety regulations
2 Identification system requirements
5 Metrology equipment control 5.1 Conditions 5.2 Calibration date and method 5.3 Handling of calibration results 5.1 Calibration period Appendix Calibration record of oxygen bomb calorimeter Appendix Measurement record of oxygen bomb calorimeter 1510 1 Scope Calibration procedure for oxygen bomb calorimeter Applicable to initial calibration, post-calibration and intermediate inspection of isothermal, adiabatic and dynamic oxygen bomb calorimeters (heat capacity range is 150·1500 J/K) 2 Overview Oxygen bomb calorimeters are used to measure the heat of combustion. Basic principle: the heat standard of a certain mother The sample is burned in an oxygen bomb in a calorimeter. The heat released makes the whole calorimeter system (negative pressure vessel, water or medium in the vessel, emulsion, mixer, calorimeter, etc.) reach the initial state temperature T, which is different from the original temperature. Then the sample is burned with the above-mentioned components for combustion measurement. The temperature is less than the original temperature of the calorimeter, and the temperature change of the calorimetric system is the same, so the heat of the substance can be obtained. The oxygen bomb calorimeter can be divided into isothermal soft bomb calorimeter (standard isothermal calorimeter) and rate bomb single bomb calorimeter (commercially known as standard isothermal calorimeter) according to the thermal principle. The calorimetric system is surrounded by a double layer of water (or other medium). When the sample is burned in the oxygen bomb of the calorimeter, the temperature of the calorimetric system rises. If the temperature change is not constant, this type of calorimeter is called isothermal calorimeter. Automatic and stepless tracking of the inner tube temperature is called an adiabatic calorimeter. Automatic oxygen bomb calorimeter (hereinafter referred to as automatic calorimeter) is simpler to operate. Except for the calibration sample and oxygen filling, the rest of the experimental process is carried out automatically. This type of endothermic calorimeter has two types: adiabatic and stirring. 3.1 Stirring heat Under certain conditions, the hot plate stirrer stirs continuously for 101min, and the temperature rise of the calorimetric system does not exceed 0.01K. 3.2 Thermoelectricity Under precipitation conditions, the combustion heat standard substance formic acid is used to calibrate the calorimeter for 5 times. The average heat capacity of the different numbers is not greater than the requirements in Table 1. 3.3 Calorific value difference Thermal variables Table 1 Thermal capacity calibration technical indicators 901 -01- 15,
Under the assumed conditions, the error between the measured calorimeter and its standard shall not exceed 6 K. 3.4 Stability of the thin point
After the initial temperature of the adiabatic calorimeter reaches equilibrium, the temperature change of the calorimetric system within 3 mi shall not exceed 0.01 K. 4 General technical requirements
4.1 Appearance requirements of calorimeters
4,1, The nameplate shall indicate the name, model, manufacturer and product! 4.12 All buttons and switches on the control panel can work normally, and all information is displayed clearly. 4.2 Internal and external tax requirements
The inner surface of the oxygen bomb shall be smooth, and the outer surface shall not have any scratches, damage, wear, rust and other defects. 4.3 Oxygen bomb requirements bzxZ.net
The inner and outer surfaces of the oxygen bomb shall not be scratched or damaged, and the cover and single screw parts shall not be worn, rusted or have other defects. At room temperature, it shall be able to withstand a water pressure test of 20MPa. 4.4 Temperature measurement system requirements
The precision thermometer has a resolution of 1K, and can also be equipped with a 5x magnification thermometer with a value of 0.01K. The thermometer should have a production license! .The work shall have the calibration certificate of the measuring and testing machine.
5 Control of measuring instruments
Measuring instruments and control include: initial calibration, subsequent calibration and intermediate calibration. 5.1 Calibration conditions
5.1.1 Calibration equipment
5.1.1.1 Standard balance, the scale is 0.1mg. The scale shall be calibrated with the calibration machine. 5.1.1.2 Balance: weighing 5kg, the scale should not exceed lk5.1.1.3 Oxygen screen: total meter quantity P10-25MPa, the positive meter quantity is 0-6MPa, and the single check is divided into 1MI and 0.2MPa.
5.11. Oxygen filling system (including oxygen reducer, pipe, etc.): production prohibition and lubrication oil Touch, if the pool is found to be contaminated, it must be washed off with an oil-producing phase lubricant and then oxygenated. The volume is -50, the graduation value is., 5.1.1.5
5.1.1.6 Autumn table: the graduation value is 0.01)
5.1.1.7 Full volume: the case is 0.-25ml, the graduation value is.1mml..5.1.1.8 Standard substances and reagent materials for determination a) Combustion heat standard item Tablet stem sodium benzoate (hereinafter referred to as benzoic acid): its mass fraction is (.7, 1.0, 1.3g-: should use the substances that have been standardized by the metrology administration and the combustion heat standard, and they have standard quality certificates. Bottle: purity is more than 99.5%.
) Standard melt: -1ul MaOH (or 0,ImalA.KOH). Prepared with pure NaOH (or KH2O), calibrated with potassium dicarbonate, accurate to 0.m/d) with indicator: acetylene solution
Ignition wire: value 0.1)--0.15m1m1, the wire and its thermal conductivity are shown in Table 2. 2 Test materials and thermal conductivity of the rat ignition
Test environment conditions
Environment humidity: [5--28°C, in the process of one test, the temperature cannot be lower than 0.5°C Environment humidity: 85%RH.
Power supply: (220_22)V, frequency (50,1)Hz, the circuit should not have strong electromagnetic and light sources, 5.1.2.4 The heat meter should be placed in a place without heat radiation and air convection. 5.1.2.5
The cooling water overflow of the adiabatic calorimeter shall be at least 3T lower than the room temperature: 5.2 Verification items and verification methods
The initial verification, subsequent verification and inspection items during use are shown in Table 3. 5.2.1
External lamp
Chu mixed chicken
Thermal identification
Flat point quick qualitative
Tracking meter
Appearance and routine inspection
Table 3 Quick determination items of calorimeter
Function of heat and heat
Typical heat and heat weight ... 1.1, 4.2, 4.4 requirements, use visual inspection to check the six real-time limit values. 5.2.2.2 According to the requirements of 4.3, check the oxygen consumption. When the oxygen pressure is filled to 3MHa, there should be no leakage. 2.3 etc. Verification method of the calorimeter. 5.2.3.1 Verification of stirring heat. Adjust the internal temperature and external temperature of the calorimeter to within 0.1 of room temperature, start the reverse stirring and record the temperature change of the calorimetric system before and after [0min]. 5.1.3.2 Heat treatment of the whole egg renaturation test: Take about 1 tablet of acid, weigh it to 0.1, and put it into the net: according to the specifications on the bullet electrode: Take a piece of metal wire, weigh it to 0.1m%, and tie its two ends to the two electrodes of the bullet respectively. Adjust the ignition wire so that it can contact with the acid in the bullet. b) Add 10m!. of steam water into the hydrogen bomb (the amount of water added should be alternating each time of calibration and determination), put the oxygen bomb into the bomb, install the expansion cover, and then connect it to the loading system, slowly fill the bomb with oxygen, and the filling time should not be less than 15. (It can also be done according to the requirements of the instrument manual), so that the pressure in the bomb reaches 3.0M. If the oxygen filling is not busy: the pressure in the bomb reaches 3.When it is 3MP, the operation should be stopped, the lysine should be replaced and the oxygen bomb should be reinstalled. ) Set the outdoor water temperature to be the same as the room water temperature, and it shall not exceed ".5K". Adjust the indoor water temperature so that the temperature will drop significantly at the end of the main program (the indoor temperature should be about 1.5K lower than the outdoor temperature during the adjustment period): the small water cover is set at 1U-2utm below the water painting (you can also operate according to the instrument manual. The indoor water should be filled with distilled water for half of the time). The amount of water taken for each calibration experiment should be alternating. d) Install the aerobic heating base ring according to the regulations, then turn on the main power, start the device, after 1iiain, when the temperature change rate of the heating disk system is selected, start to cut off the temperature, record the temperature every 30 conditions, read to 0.001K, and read 1U times in total. Turn on the ignition switch at the same time as the 11th reading. The temperature is the initial temperature of the period (). +The temperature reading of the period will still be recorded every 30s. When the temperature rise is greater than 0.5K, read 0.1K; when the 30s is 0.1-0.5K, the number will be incremented to 0.01K: when the temperature rise is less than 0.1K, the accuracy will be 0.WIK: when the main period temperature reaches the maximum value, the first temperature that starts to drop is the end of the main period (!), the store will conduct unshot product chain payment, and the temperature will be recorded every 30s. The reading price is EUR
) After the test, exhaust the gas in the bomb, wash the bullet head, the inner frame, the inner wall of the bomb with hot water, collect 200ml of washing liquid, heat it in the center, add 3-5 drops of cooling agent, titrate with 1r.V>「(or .Ine./K(H) standard solution), record the consumed standard volume, weigh the maximum volume and record the remaining volume after combustion. Wind ignites some quality, to compensate! (only the manual does not require this item!
card: add if found loss or internal area staff: experimental degree. [】 wider up 4 times, a total of 5 times, then the formula: 1 calculate the heat capacity, and calculate the half-average heat space to the length difference, F:mo+mior+vOz
where: E
heat penetration, J/K:
benzene acid 3:
Benzene acid standard calorific value: J/2
Ignition quality (the quality difference of the wire before and after ignition, the calorific value of the wire, J/
The volume of the standard solution consumed in the titration, ratio: the heat of acid formation within 0.1r period is 5.9/ml. The calorimetric system after the discharge is not expected, K;
The average graduation value of the calorimeter (using the head thermometer H-1). 4t = [trI h) (tr I: a
ir and h..
Wuzhong: V and V
-three-phase initial pollution flow river, K;
The image at the private temperature point is positive, K;
Its thermal system and the heat of the ring are corrected, K: -
V,-Vurta-t,
Initial and wooding period temperature change, K/3s1
Average temperature during accumulation and final period, K:
--Turpan speed to take virtual change number:
Temperature readings in order during the harvest period
: If computer limited word system is used, then the measurement panel will automatically calculate and 5.2.3.3 Thermal reading difference verification
Take about 0.7g and 1.35 tea coins of acid tablets and connect 5.2.3.2 book to operate, according to formula (4! Calculate the heat of rice acid:
EHA- - mIQI -VQ?
where, is the heat average heat quantity, 1,
According to formula (5), its calorific value error,
Formula: 2Q——calorific value difference, 1/g:
Q: Q -Q:
Measured mean calorific value of benzene, J/g
Qs——Standard calorific value of formic acid, J
5.2.4 Verification method of adiabatic calorimeter
5.2.4.1: Verification of equilibrium point stability
After the initial temperature of the adiabatic calorimeter reaches equilibrium, record the temperature change of the calorimetric system for 3min. 5.2.4.2 Verification of calorimetric repeatability
a) Measure formic acid and install the load in the same way as 5.2.3.2. Adjust the internal water temperature to 1-3K higher than room temperature and weigh to 6) Turn on the main power of the calorimeter, start the agitator, circulation system and the heating switch for external temperature interval, adjust the cooling volume and the power on the calorimeter panel: in about 1min, the recorded temperature should reach equilibrium. Design: Foreign merchants use water containing M(X to make it feel large and release it to about 100%. The calorimeter is usually balanced in the future. In the actual situation, the environment does not change. There is no need to turn the balance potentiometer on the panel. c) After the calorimeter reaches equilibrium, read the internal temperature (cm3) and start the bucket leaf at the same time. Read the internal flow rate (2) 3min after ignition. The average of the two temperatures is the average temperature of the period (t: 12rain after ignition, read the internal flow rate (), read the internal temperature (a) 3um apart, and the average of the last two temperatures is the average temperature of the final period (): The time between the initial and the final period can be classified according to the technical regulations. c) After the experiment is completed, the oxygen-free operation is the same as 5.2.3.2). Repeat the above test 4 times, and calculate the heat capacity according to the public test (6) to calculate the average heat equal amount range.
Q+ mQ1 -VQ2
F\Ht+h-+ho
Wu Zhong: - initial level and surplus ammonium, K:
half mean value of operation period: K.
5.2.4.3 Calorific value error verification
Take about 0.7g and 1.3g of formic acid tablets and perform the operation according to the steps of 5.2.4.2 respectively. Calculate the calorific value of formic acid according to formula (71) and then calculate the average value and compare it with the standard value. Q
E(t + h)-(ta + h-miQ 5.2.5 Automatic calorimetric verification method 5.2.5.1 Verification of heat capacity repeatability Weigh the lysine and install the oxygen bomb according to the above method, then follow the technical instructions to determine the heat capacity measurement program, input the necessary data to the computer, and automatically calculate the heat capacity after the experiment. Repeat the test 4 times, calculate the average heat capacity and report the error. 5.2.5.2 Determination of calorific value error According to the technical instructions, select the calorific value determination program, determine the calorific value of 0.7g and 1.3g lysine respectively, calculate the daily average calorific value, and compare it with the standard value. 5.3 Mandatory results of the test
After the test, the thermometer that meets the requirements of this regulation shall be issued with a certificate of verification. If it does not meet the requirements, a new verification result notification shall be issued, and the non-qualified items shall be pointed out.
5.4 Verification period
The verification period shall not exceed 2 years.
Appendix 4 Oxygen bomb thermometer verification record
Original record number
Instrument name
Equipment number
Technical number of material
Sample level number
Ambient temperature
Certificate screening number
External inspection:|| tt||Stirring heat test delay:
Heat capacity test:
Baking value error:
Test period
Measurement item date
Original record
Ambient temperature
Volume
Heat volume (JK)
To obtain calorific value: (Jg
Flood plant number
Testing unit
Heat value (Q)
Inner water quality
Circulation degree
Heat: g
Tester
Appendix B
Isothermal thermometer measurement record sheet
Combustible capacity (or calorific value)
Standard material formic acid shear value ()-
Ignition wire calorific value (Q
Standard solvent reduction village equivalent to [
Measurement record
Environmental humidity
Absorption/()
And standard production potential
Tester
Benzene formic acid mass distance (m)
Ignition wire cover
Consumption of standard solvent (V)
Unstandardized temperature
Toughness K
Calculation of potential exchange
Calculation of heat rate temperature rise
at = (t. + h.) - (tn+ in 26 heat set (or hot sale) Xun bucket calculation
mQ-m+V
Q_FHAL-mQ-VQ:
Pattern date
Inspector
This-
Inspector
Test items
Original number
Underground temperature
Adiabatic calorimeter code quantity record table
Heat research quantity calorific value)
Annotated substance Benzoic acid calorific value (Q)
Wire calorific value ()
Standard melt wave rolling equivalent (center:)
1 Appearance inspection
2 Balance point stability test
3 Heat according to the system F operation: calculation god
(i- ho)
(,+) -
Calculation of heat capacity F (or calorific value Q)
mU + m.Qi! VQ?
Closed-mouth period
Environmental sensitivity
Relative mass of standard substance in benzene (m)
Leading halogen
Consumable standard solution (1)
Tester
Tester
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