CN102591214A - Cooling water cutoff protection device of azotometer - Google Patents

Cooling water cutoff protection device of azotometer Download PDF

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Publication number
CN102591214A
CN102591214A CN2011100083922A CN201110008392A CN102591214A CN 102591214 A CN102591214 A CN 102591214A CN 2011100083922 A CN2011100083922 A CN 2011100083922A CN 201110008392 A CN201110008392 A CN 201110008392A CN 102591214 A CN102591214 A CN 102591214A
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azotometer
cooling water
water flow
time
protection device
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夏瑛
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SHANGHAI PEIOU ANALYTICAL INSTRUMENTS CO Ltd
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SHANGHAI PEIOU ANALYTICAL INSTRUMENTS CO Ltd
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Abstract

The invention relates to a cooling water cutoff protection device of an azotometer, which is included in a control unit of the azotometer, and heating is stopped and an alarm is given when cooling water is cut off. The cooling water cutoff protection device of the azotometer preferably records residual distillation time and breaker point time when the cooling water is cut off, and stops heating distillation and a gives a sound alarm; and after the cooling water is restored, the alarm is eliminated, a distillation power supply is switched on, and the continuous distillation time is the sum of the residual distillation time and the time compensated by evaporator cooling caused by water cutoff time. Compared with the prior art, the invention has the following advantage that after the cooling water is subjected to cutoff protection, a sample can be continuously used and can be avoided being discarded.

Description

Azotometer cooling water flow stoppage protection device
Technical field
The present invention relates to be used for the Instrument technology field of food, feed, soil, chemical fertilizer survey nitrogen content, be specifically related to azotometer cooling water flow stoppage protection device.
Background technology
The fields such as food processing, nutrition health, agricultural production, feed industry that are determined at of protein content all have great importance, and in processing, research, production and the trade in these fields, are paid much attention to.What be used widely at present is that speed is fast, the check nitrogen content that cost is low and the azotometer of protein content, and its principle of work is to adopt the method for measuring nitrogen pool in compound or the potpourri; Promptly having under the condition of catalyzer; With the nitrated sample of the concentrated sulphuric acid, organic nitrogen all is transformed into inorganic ammonium salt, under alkali condition, ammonium salt is converted into ammonia, distillates cooling, also absorbs for excessive borate with water vapor then; With the standard acidometric titration, just can calculate the nitrogen amount in the sample again; Because the protein nitrogen content is more constant, can calculate protein content by its nitrometer.The cooling of ammoniacal liquor is the important step of distillation in said method, if the chilled water cutout will make ammonia temperature raise and continue distillation, ammonia is overflowed and made detectable concentration reduce, and causes the sample data error huge, draws error result.Therefore cooling water flow stoppage protection is the important protection part of azotometer, and existing high-end azotometer generally possesses this function, and it is through cutting off heating and reporting to the police to tell the checker this distillation failure when chilled water stops, and data can not be used; Yet after cutting off the water supply, sample has just been scrapped, and also needs about 2 hours and make sample again.
Summary of the invention
The object of the invention be exactly in order to overcome in the existing azotometer behind the cooling water flow stoppage protection that sample such as scraps at defective and after a kind of cooling water flow stoppage protection is provided sample can also continue to use, thereby improve the efficient of measuring nitrogen content and the azotometer cooling water flow stoppage protection device of the cost that economizes in raw materials.
The object of the invention can be realized through following technical scheme: azotometer cooling water flow stoppage protection device is included in the control module of this azotometer, when chilled water stops, cuts off heating and warning.
Said azotometer cooling water flow stoppage protection device writes down residue distillation time, breaker points time when chilled water stops, cut off to add thermal distillation audible alarm simultaneously; Continue the back at chilled water and eliminate and report to the police, connect the distillation power supply, continue distillation time and be the time that evaporator cools that described residue distillation time adds that the time of cutting off the water supply causes compensates.
Said control module also comprises LCD MODULE, and said azotometer cooling water flow stoppage protection device also shows reason on the screen of said LCD MODULE in audible alarm.
Said control module also comprises 6 key board modules.
Said 6 key board modules are film soft-touch type keyboard.
Said control module also comprises security protection module, and this security protection module comprises that lack of water is reported to the police, scarce alkali is reported to the police, acid deficient is reported to the police, the condensation lack of water is reported to the police, report to the police and safety door position alarm module in nitrated pipe position.
Said control module also comprises the control module of carrying out temperature, control, communication, alerting signal processing.
Said control module also comprises control module and the security protection module that carries out temperature, control, communication, alerting signal processing, and this security protection module comprises lack of water warning, scarce alkali warning, acid deficient warning, the warning of condensation lack of water, the warning of nitrated pipe position and safety door position alarm module.
Compared with prior art, beneficial effect of the present invention is following:
1, azotometer cooling water flow stoppage protection device can guarantee that chilled water cutout back sample can continue to distill and the same condition with normal distillation, makes again the required time of sample in that sample has not also been saved when scrapping.
2, azotometer cooling water flow stoppage protection device also can show reason on the screen of LCD MODULE in audible alarm, thereby the operator can carry out handled as early as possible, has improved work efficiency.
Description of drawings
Fig. 1 is the azotometer front view;
Fig. 2 is the azotometer left view;
Fig. 3 is the azotometer rear view;
Fig. 4 is an azotometer cooling water flow stoppage protection schematic diagram of device;
Fig. 5 is an azotometer control module synoptic diagram;
Wherein: 1, nitrated conduit saddle, 2, safety door, 3, liquid-collecting bottle, 4, operation interface, 5, power switch; 6, air scoop, 7, the alkali lye import, 8, the dilution import, 9, the distilled water import; 10, acid solution import, 11, the electrical heating view window, 12, supply socket, 13, fuse; 14, liquid level sensor interface, 15, cooling water inlet, 16, coolant outlet, 17, the outlet of distilled water raffinate.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
Embodiment:
Shown in Fig. 1-3, the nitrated conduit saddle 1, safety door 2, liquid-collecting bottle 3, operation interface 4 and the power switch 5 that are positioned on the main-vision surface plate are arranged on the said azotometer; Be positioned at air scoop 6, alkali lye import 7, dilution import 8, distilled water import 9, acid solution import 10 and electrical heating view window 11 on the panel of the left side; Be positioned at supply socket 12, fuse 13, liquid level sensor interface 14, cooling water inlet 15, coolant outlet 16 and distilled water raffinate outlet 17 on the back panel.Said azotometer comprises control module and the nitrated unit that links to each other successively, distills unit, condensing unit, liquid collecting unit, the azotometer cooling water flow stoppage protection device that cuts off heating and report to the police when being included in the chilled water cutout in the said control module.
Said azotometer cooling water flow stoppage protection schematic diagram of device is as shown in Figure 4, and it writes down residue distillation time (T), breaker points time when chilled water stops, and cuts off to add thermal distillation audible alarm, screen display reason simultaneously; Continue the back at chilled water and eliminate and report to the police, connect the distillation power supply, continue distillation time and be the time (t) that evaporator cools that described residue distillation time (T) adds that the time of cutting off the water supply causes compensates.In the azotometer use, come off to cause and cut off the water supply when cooling water pipe, the instrument audible alarm, the screen display checker that " please open chilled water " hears that chimes of doom arrives in by the instrument simultaneously, finds that water pipe comes off, and connects water pipe immediately, opens the water source; This moment, chimes of doom stopped, and small character shows " Y " below the screen display " continuations ", and the checker is by corresponding " Y " key, instrument continues to distill, and finishes up to distillation time; Ensured the safety of sample.
Said control module is as shown in Figure 5, also comprises 6 key board modules, and this 6 key board module is a film soft-touch type keyboard; Said control module also comprises control module and the security protection module that carries out temperature, control, communication, alerting signal processing, and this security protection module comprises lack of water warning, scarce alkali warning, acid deficient warning, the warning of condensation lack of water, the warning of nitrated pipe position and safety door position alarm module.
The concrete use as follows:
1, the preparation of chemical reagent: NaOH (NaOH) solution of preparation 30%~40% adds in the lye tank for 3~5 liters, bung tightened, and preferred concentration 35%, this moment, solution was difficult for crystallization, blocking pipeline after room temperature changes; Prepare 2% boric acid (H 3BO 3) 3~5 liters of solution add in the boric acid liquid feeding bucket, mix, bottle cap is tightened; Preparation hydrochloric acid (HCl) vs, solubility is decided according to the content of sample, is generally 0.1 volumetric molar concentration (M), and with 0.05~0.02 volumetric molar concentration, concentration needs accurately to demarcate to the low content sample.Preferred nitre boils sample and need have sulfuric acid (H 2SO 4), copper sulphate (CuSO 4), glazier's salt (K 2SO 4), when sample size takes by weighing 0.5~1 gram, add concentrated sulphuric acid 8ml~10ml, add copper sulphate: glazier's salt is 1: 3 potpourri 6 grams.
2, operation interface function and the respective operations in the said control module:
Instrument adopts controlled by single chip microprocessor, and the large-screen lc screen shows that by prompting operation, simple and convenient after the energized, control is reliable.Film soft-touch type keyboard, water proof and dust proof, the life-span is lasting.
Before opening power switch device, check whether distilled water, alkali lye, acid solution, dilution, chilled water, liquid-collecting bottle etc. connect.Open power switch device again, open the chilled water tap, select the program sequence number of setting, by starting.
(1) start display interface: screen display instrument model and manufacturer; The start energising detects the cucurbit liquid level automatically, is lower than normal water level and adds water automatically, adds water overtime (gave tacit consent to 2 minutes, the time is adjustable), alarm.
(2) show use reagent interface: show boric acid, alkali lye, distilled water, dilution situation; Corresponding keypad function symbol is: _ _ invalid, _ _ invalid, affirmation; Press acknowledgement key and continue next step, if lack a certain reagent, liquid crystal display alarm.
(3) interface seven: prompting input correct time and date (this information will be preserved with service data); Corresponding keypad function symbol is: ← to the right, → left ,+the increase circulation ,-minimizing circulates,
Figure BSA00000419218500042
confirms; Button is revised; 2000-2099, the 1-12 month, 1-31 day, instrument can write down stop time; Press acknowledgement key and continue next step.
(4) operations interface (interface eight): show sample test, parameter setting, check sample, manual mode and EOT; Corresponding keyboard symbol is: R resets, ← upwards, → downwards, _ _ invalid, confirm (next step); According to interface selection operation project, use for the first time, advanced line parameter setting; When operation, multi-group data can be set simultaneously, sequence number can be revised, and total the preservation remembered 0-99.
(5) sample parameters is provided with interface (interface 16): show sample numbering (00-99), adds acid time (00.0-30.0 second), dilution time (00.0-30.0 second), add-subtract time (00.0-30.0 second) and degree of heat (100/80/60/50%) at distillation time (00.0-99.0 branch); Corresponding keyboard symbol is: R returns, ← upwards, → downwards ,+increase circulation ,-reduce circulation,
Figure BSA00000419218500044
confirms; Continue to return a last menu by return key, carry out sample test.
(6) sample test interface ( interface 11,12,13): display setting date and time, sample number into spectrum (00-99) add acid time (00.0-30.0 second), distillation time (00.0-99.0 branch), dilution time (00.0-30.0 second), add-subtract time (00.0-30.0 second) and degree of heat (100-50%); After adding acid, next step distillation operation automatically, add dilution after, automatically next step, add alkali after, countdown to be distilled finishes; Corresponding keyboard symbol for R reset, _ _ invalid, R/P operation/time-out; The general parameter sequence number that shows last setting also can be selected the sample test of different sequence numbers.
Instrument test example interface (interface nine): display setting date and time; Sample number into spectrum (00-99); Add the acid time (00.0-30.0 second), distillation time (00.0-99.0 branch), dilution time (00.0-30.0 second), add-subtract time (00.0-30.0 second) and degree of heat (100-50%); Wherein add and subtract x and stop y second for s/ time, x=3 y=2 is preset for acquiescence, but keyboard is revised; Add when just beginning distillation after the acid and adding dilution and add alkali and time operation, do countdown and show; Corresponding keyboard symbol is: R resets, _ _ invalid, ← return interface eight, → existing parameter (interface ten),
Figure BSA00000419218500051
confirm operation (interface 11); Finish back alarm automatically, show and preserve test parameter (0-999 group).
(7) preserve test parameter interface (interface 14): the display setting date and time, sample number into spectrum (00-99), sample stores sequence number (000-999 adds 1 automatically), acid (S), distillation (M), dilution (S), alkali (S), power % etc.; Keypad function symbol is: R resets, _ _ invalid, F returns continuations, master menu is returned in affirmation; Continue former sequence number sample operation by return key, return master menu by acknowledgement key; Select to finish test, instrument is preserved parameter and the time after the start, and shutdown finishes.When starting shooting again, press aforesaid operations, in the optional sample of checking of master menu, 0-999 kind.
(8) check and transfer example interface (interface 15): with forms mode show sample numbering and corresponding sour S thereof), the numerical value situation of distillation (M), dilution (S), alkali (S), power % etc.; Corresponding keypad function symbol is: R resets ,+following one page ,-page up,
Figure BSA00000419218500053
confirm (interface eight); Through this interface operation, can check and transfer the data of having done, show a last step menu sequence number and back parameter; In master menu player dynamic model formula, manually can add all ingredients or check each road reagent and operation valve working condition.
(9) interface (17) are manual mode interface (by the corresponding key of each numeral, can manually carry out the interpolation of each reagent or the detection of each operation valve); Show its ON/OFF situation successively; Corresponding keypad function symbol is: R returns, 5 heating ON/OFF, 4 add water ON/OFF, 3 and add alkali ON/OFF, 2 and add dilution ON/OFF, 1 and add sour ON/OFF.
(10) interface three, four, five, six is the improper prompting of liquid level interface: the self check situation of display instrument, and self check this moment, whether mug liquid level, dilution liquid level, boric acid liquid level, alkali lye liquid level, distilled water liquid level be normal; Report to the police when improper, after handling abnomal condition well, alerting signal disappears automatically; Directly next step setting of alarm free.
(11) subsidiary function interface:
Display interface when (11.1) lacking liquid; Demonstration please add acid (alkali, dilution), by confirming i.e. completion.
(11.2) check oneself and the interface is set (control through special key, the user does not change easily, changes if need; Must under the guidance of producer, carry out): show moisturizing time-delay T (0.0-2 second), preheating T (20.0-30.0 second), the overtime T1 of start moisturizing (1-2 branch; Surpassing setting-up time reports to the police), the overtime T2 of moisturizing in the operational process (00.1-02.0 second, surpass setting value and report to the police); Liquid feeding T interval time adds alkali interval time (stop yS xS/ time, x, y value are predeterminable).
(11.3) door switch is provided with the interface and (is provided with through special key; The user does not change if need to change easily, must under the guidance of producer, carry out): show that successively dilution liquid level, alkali lye position, acid solution position, water flow switch, sample are on the throne, the ON/OFF situation of door switch; Switch is a normally closed switch." open " expression: switching function exists, and " pass " expression: switching function does not exist, and promptly switch has been broken and selected time item also can work.
(11.4) temperature alarming is provided with the interface (be provided with through special key, the user does not change easily! ): show XX ℃ of observed temperature, design temperature XX ℃; Corresponding keyboard functor is:--4,--1; Before powering on, machine pins 1 and 4 keys simultaneously.
(11.5) the factory reset interface (is provided with user-operable when being necessary through special key! ): show whether factory reset, realize through selecting " being ", " denying ".
Is (11.6) sample, door, the interface when chilled water lacks: show sample put well? Does door closes get well? Is chilled water opened? By confirming to carry out next step operation.
Is (11.7) trouble shooting interface: demonstration please be checked: the distilled water raffinate fastened? Are Distilled water bucket lack of water water, acid, alkali bottle cap tightened? Does Distilled water bucket leak? Carry out next step operation by solution.
3, the test of sample: at first be the preparation of sample, sample take by weighing the nitrogen content in the considered sample, the nitrogen content in the sample is high, it is less then should to take by weighing sample size; If the nitrogen content of sample is low, it is some more to take by weighing sample size.The standard acid of generally choosing 0.1 volumetric molar concentration is as Titrable acid, and the nitrogen content that takes by weighing in the sample is generally 2~50 milligrams of nitrogen optimums.When sample is nitrated, adds sulfuric acid and get final product for about 8~10 milliliters, copper sulphate, glazier's salt addition are decided according to industry sample situation.Treat nitrated fully after, take off cooling, in nitrated pipe, add 30 milliliters of left and right sides distilled water diluting samples and release heat, cool off subsequent use.The relation of choosing the nitrogen content in titrimetric standard acid and the working sample is as shown in the table:
The volumetric molar concentration of titrimetric standard acid Nitrogen content in the working sample
0.02 volumetric molar concentration 1~20 milligram of nitrogen
0.1 volumetric molar concentration (routine) 15~100 milligrams of nitrogen
0.15 volumetric molar concentration 30~160 milligrams of nitrogen
Main process and reaction equation are following in the azotometer inventive principle in the foregoing description:
Nitrifying process: the amine root in the organism sample is at heat-flash and CuSO4, dense H 2Under the SO4 effect, nitrated generation (NH 4) 2SO 4Reaction equation is: 2NH 2+ H 2SO 4+ 2H=(NH 4) 2SO 4(CuSO wherein 4Make catalyzer).
Still-process: sample and alkali effect in the kjeldahl determination device, through regularly, decide power and distill and discharge NH 3, NH 3Mixing is cooled to suitable low temperature through condensate water and is collected in H with water vapor 3BO 3In the solution.
Reaction equation is: (NH 4) 2SO 4+ 2NaOH=2NH 3+ 2H 2O+Na 2SO 4
NH 3+4H 3BO 3=(NH 4) 2B 4O 7+5H 2O
Titration process: with the H of concentration known 2SO4 (or HCI) standard solution titration, the amount that consumes according to HCI calculates the content of nitrogen, multiply by corresponding conversion factor then, both the sample protein content.
Reaction equation is: (NH 4) 2B 4O 7+ H 2SO 4+ 5H 2O=(NH 4) 2SO 4+ 4H 3BO 3
(NH 4) 2B 4O 7+2HCl+5H 2O=2NH 4Cl+4H 3BO 3

Claims (8)

1. azotometer cooling water flow stoppage protection device, it is characterized in that: said azotometer cooling water flow stoppage protection device is included in the control module of this azotometer, when chilled water stops, cuts off heating and reports to the police.
2. azotometer cooling water flow stoppage protection device according to claim 1 is characterized in that, said azotometer cooling water flow stoppage protection device writes down residue distillation time, breaker points time when chilled water stops, and cuts off to add thermal distillation audible alarm simultaneously; Continue the back at chilled water and eliminate and report to the police, connect the distillation power supply, continue distillation time and be the time that evaporator cools that described residue distillation time adds that the time of cutting off the water supply causes compensates.
3. azotometer cooling water flow stoppage protection device according to claim 2; It is characterized in that; Said control module also comprises LCD MODULE, and said azotometer cooling water flow stoppage protection device also shows reason on the screen of said LCD MODULE in audible alarm.
4. according to claim 1,2 or 3 described azotometer cooling water flow stoppage protection devices, it is characterized in that said control module also comprises 6 key board modules.
5. azotometer cooling water flow stoppage protection device according to claim 4 is characterized in that, said 6 key board modules are film soft-touch type keyboard.
6. according to claim 1,2 or 3 described azotometer cooling water flow stoppage protection devices; It is characterized in that; Said control module also comprises security protection module, and this security protection module comprises that lack of water warning, scarce alkali are reported to the police, acid deficient is reported to the police, cools off lack of water warning, the warning of nitrated pipe position and safety door position alarm module.
7. according to claim 1,2 or 3 described azotometer cooling water flow stoppage protection devices, it is characterized in that said control module also comprises the control module of carrying out temperature, control, communication, alerting signal processing.
8. azotometer cooling water flow stoppage protection device according to claim 6 is characterized in that, said control module also comprises the control module of carrying out temperature, control, communication, alerting signal processing.
CN2011100083922A 2011-01-14 2011-01-14 Cooling water cutoff protection device of azotometer Pending CN102591214A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114414724A (en) * 2022-01-12 2022-04-29 广东省科学院测试分析研究所(中国广州分析测试中心) Novel water-free azotometer

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86209078U (en) * 1986-11-14 1987-10-03 陈炳焕 Rotary nitrogen fixation instrument
DE19653215A1 (en) * 1996-01-23 1997-07-24 Buechi Lab Tech Nitrogen content determination apparatus for organic samples, e.g. proteins
CN101294914A (en) * 2007-04-27 2008-10-29 李立华 Computer full-automatic Kjeldahl determination device
CN201569646U (en) * 2009-12-03 2010-09-01 汤国型 Three-control azotometer
CN201628710U (en) * 2010-04-02 2010-11-10 杨广超 Water level alarm and condensate circulating device of azotometer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86209078U (en) * 1986-11-14 1987-10-03 陈炳焕 Rotary nitrogen fixation instrument
DE19653215A1 (en) * 1996-01-23 1997-07-24 Buechi Lab Tech Nitrogen content determination apparatus for organic samples, e.g. proteins
CN101294914A (en) * 2007-04-27 2008-10-29 李立华 Computer full-automatic Kjeldahl determination device
CN201569646U (en) * 2009-12-03 2010-09-01 汤国型 Three-control azotometer
CN201628710U (en) * 2010-04-02 2010-11-10 杨广超 Water level alarm and condensate circulating device of azotometer

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114414724A (en) * 2022-01-12 2022-04-29 广东省科学院测试分析研究所(中国广州分析测试中心) Novel water-free azotometer
CN114414724B (en) * 2022-01-12 2024-02-02 广东省科学院测试分析研究所(中国广州分析测试中心) Novel water-free azotometer

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Application publication date: 20120718