CN102393466A - Primary amino radical tester - Google Patents
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- CN102393466A CN102393466A CN2011102494801A CN201110249480A CN102393466A CN 102393466 A CN102393466 A CN 102393466A CN 2011102494801 A CN2011102494801 A CN 2011102494801A CN 201110249480 A CN201110249480 A CN 201110249480A CN 102393466 A CN102393466 A CN 102393466A
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Abstract
The invention discloses a primary amino radical tester, which is obtained by improving a paradigm amino acid tester, is mainly used for measuring the primary amino radical content of proteins, and is popularized and application to the measurement of the primary amino radical content of various organic compounds. The tester mainly comprises a reaction part, a gas measuring part, a gas washing part and a recovering part, and has the characteristics of rapidness, accuracy, cleanliness and the like.
Description
Technical field:
The invention belongs to chemical analysis test instrument and equipment field, relate to a kind of instrument---primary amino radical analyzer of measuring protein primary amino radical content (comprising collagen polypeptide, each seed amino acid) that is mainly used in.
Background technology:
The method that is used for measuring protein primary amino radical group content at present all has ninhydrin colorimetry, TNBS colourimetry, micellar electrokinetic chromatography method, formaldehyde method, Van Slyke's method, vapor-phase chromatography.Wherein, triketohydrindene hydrate colorimetric and TNBS colorimetric belong to AAS, all have instrument error.In addition, in ninhydrin colorimetry, the depth of the time length of heating colour developing and colour developing back color all can cause error; TNBS colourimetry selectivity is very strong, and main and lysine epsilon-amino reacts, can not quantitatively whole primary amino radicals.In the formaldehyde method, also there is further the subsidiary reaction with the primary amino radical condensation in methylol compound, influences accuracy of measurement.In addition, formaldehyde receives the generation oxidation that influences of external environment to become formic acid owing in depositing process easily, formic acid meeting additive decrementation NaOH in titration process, thus make measurement result higher.Though chromatography so has high sensitivity, but instrument and equipment is had relatively high expectations, for example: required stainless steel reaction device processing request is high and involve great expense in the vapor-phase chromatography.In the Van Slyke's method use measuring period long, experimental implementation is complicated, it is bigger that experiment is influenced by ambient temperature.
Existing normal form amino acid determining instrument mainly is made up of reaction unit, amount device of air and air-washer three parts.Wherein reaction unit and air-washer are respectively integral structure, bring many inconvenience to cleaning.Former normal form amino acid determining instrument needs special-purpose support to fix, and it is big to take up room.Test receives surrounding environment influence bigger, can not measure under the low temperature.The normal form amino acid determining instrument does not carry out Unified Treatment to waste gas, waste liquid, and environmental pollution is serious.
Summary of the invention:
To the deficiency of prior art, the purpose of this invention is to provide a kind of primary amino radical acidity test appearance with and method of application.
The present invention is principle with the Van Slyke's method, on the basis of normal form amino acid determining instrument, designs a kind of quick, simple, accurate, clean primary amino radical analyzer.The reactive moieties of analyzer (I) includes magneton (9), has water-bath chuck (4) and magnetic agitation (10), and reactor (1) bottom is flat design.The gas washing part (III) of analyzer includes magneton (29), is furnished with magnetic agitation (30), and gas washing hemisphere (27) bottom is flat design.This device can be used for the measurement of primary amino radical group in protein, gelatin and the micro-amino acid.
A kind of primary amino radical analyzer; Form by reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV); It is characterized in that; Reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV) connect successively, and the exhausr port and the leakage fluid dram of reaction unit (I), amount device of air (II), air-washer (III) all are connected on the recovery section (IV).
Preferably, described reaction unit (I) comprises reactor (1), charge pipe (2) and three-limb tube (14).Preferably, three-limb tube (14) has cock (15), and cock (15) is positioned at three-limb tube (14) intersection, is used for the trend of adjustments of gas in three-limb tube (14).
Preferably, described reactor (1) top is ground (12), and the bottom is flat, has water-bath chuck (4), and is as shown in Figure 1.A thin neck glass tube (7) and a downward drainage conduit (11) upwards arranged at reactor (1) bottom; One end of thin neck glass tube (7) connects charge pipe (2), and the other end passes chuck (4) and connects with reactor wall (5); Drainage conduit (11) is passed chuck (4) and is connected with reactor wall (5), is used for the discharge of reactor (1).Preferably, contain two interfaces (6) on reactor jacket (4) outer wall, be used for the communication loop water-bath.Preferably, reactor (1) contains magneton (9), the supporting magnetic agitation in bottom (10).
Preferably, described reaction unit (I) comprises two charge pipes---first charge pipe (2) and second charge pipe (3).Preferably, first charge pipe (2) and second charge pipe (3) bottom are thin neck glass tube, and first charge pipe (2) is 25～35ml, and second charge pipe (3) is about 10～20ml.Reaction unit (I) comprises two thin neck glass tubes, and the first thin neck glass tube (7) and the second thin neck glass tube (8) connect first charge pipe (2) and second charge pipe (3) respectively.
Preferably, three-limb tube (15) is connected with reactor top ground (12) through the grinding port plug (13) of thin neck glass tube one end, and the other end of three-limb tube (15) links to each other with inclined hole stop,threeway (19) through thin neck bend pipe (17).
Air-washer (III) comprises gas washing hemisphere (27) and buffering ball (26); Gas washing hemisphere (27) and buffering ball (26) are connected with inclined hole stop,threeway (19) through thin neck glass connecting pipe (23).Preferably, gas washing hemisphere (27) radius is 100～150mm, and buffering ball (26) radius is 80～100mm.
Preferably, gas washing hemisphere (27) top connects thin neck glass tube (24), is used for the gas turnover; The bottom has a downward glass tube (25) and is used for discharge opeing, and have one 90 ° upwards bend pipes (28) be used to connect buffering ball (26).Gas washing hemisphere (27) is flat, includes magneton (29), supporting magnetic stirring apparatus (30).
Described retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33).Preferably, returnable bottle (33) is furnished with the plug (36) that contains two glass tubes (34), (35).
Reactor of the present invention (1) is furnished with water-bath chuck (4); The bottom connects two charge pipes; First charge pipe (2) and second charge pipe (3); Top ground (12) is connected with three-limb tube (14) through the grinding port plug (13) of thin neck glass tube one end, and three-limb tube (14) other end links to each other with inclined hole stop,threeway (19) through thin neck bend pipe (17), and eudiometer tube (20) bottom connects level ball (21) (emulsion tube (22) length is 1.5 times of eudiometer tube (20)) through emulsion tube (22); Eudiometer tube (20) top straight tube (18) connects gas washing hemisphere (27) through connecting pipe (23), and the 90 ° of bend pipes (25) that make progress in gas washing hemisphere (27) lower end connect buffering ball (26).Three-limb tube gas outlet (16), reactor discharging tube (11), gas washing hemisphere discharging tube (25) all are connected with four-way connecting pipe (31) through silicone tube (having tongs on the silicone tube of discharging tube (11), (25) mouth), are connected on the retracting device (IV) through silicone tube (32) again.
The water-bath chuck (4) of reactor of the present invention (1) connects constant temperature water bath, in order to the conditioned reaction temperature; Reactor (1) includes magneton (9), and the bottom is furnished with magnetic agitation (10), can reaction speed through regulating stirring rate.Gas washing hemisphere of the present invention (27) includes magneton (29), and the bottom is furnished with magnetic agitation (30), regulates gas washing speed through regulating stirring rate.
The present invention also provides the method for application of said uncle's ammonia quantitative instrument, comprises the following steps:
Carry out preliminary work before the use of the present invention earlier, each interface of good seal, reactor discharging tube (11) and gas washing hemisphere discharging tube (25) clip with tongs.At first inject deionized water from level ball (21), eudiometer tube (20) is filled with deionized water after, turn eudiometer tube cock maintenance dose tracheae (20) is full of water state.Then with gas washing liquid (potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400ml); Pour into from surge flask (26); Fill with gas washing hemisphere (27) to eudiometer tube cock (19) when locating, turn eudiometer tube cock (19) makes eudiometer tube (20) communicate with three-limb tube (14).Improve level ball (21), eudiometer tube (20) is filled with deionized water to three-limb tube cock (15) locate.Turn three-limb tube cock (15) makes reactor (1) communicate with retracting device (IV) through three-limb tube gas outlet (11), and turn eudiometer tube cock simultaneously (19) is to horizontal direction, the closing capacity tracheae.Be put in lower to level ball (21), equal full of liquid in gas washing hemisphere this moment (27) and the eudiometer tube (20), and and isolate from outer air.Open circulator bath and magnetic agitation (10).
Add the about 20～30ml of glacial acetic acid from first charge pipe (2) earlier during test sample of the present invention, then add 40% the about 20～30ml of sodium nitrite in aqueous solution, closed first charge pipe (2) and second charge pipe (3).Reactor (1) internal reaction generates NO or NO
2Gas keeps 5～8min, the interior air of emptying reactor (1).Turn three-limb tube cock (15), closed reactor (1).Open first charge pipe (2) and second charge pipe (3); Producing gas in the reactor (1) drives liquid out of from first charge pipe (2) and second charge pipe (3); After gas is driven out of fully in the thin neck of first charge pipe (2) and second charge pipe (3) bottom, closed first charge pipe (2) and second charge pipe (3).Turn three-limb tube cock (15) and eudiometer tube cock (19) only communicate reactor (1) with eudiometer tube (20), keep reactor (1) interior gas inlet tracheae (20).In first charge pipe (2), fill with deionized water, fluid-tight.In second charge pipe (3), add testing protein solution, slowly open charge pipe (3) cock, make the slow inflow reactor of liquid to be measured (1), and wash second charge pipe (3), with the n-amyl alcohol fluid-tight with small amount of deionized water.Closed second charge pipe (3) during reinforced the end.In the course of reaction, when gas in the eudiometer tube (20) surpasses the eudiometer tube venturi portion, improve level ball (21) rapidly, turn eudiometer tube cock (19) is caught up with gas into gas washing hemisphere (27).After gas is caught up with only, turn eudiometer tube cock (19), closed gas washing hemisphere (27) makes eudiometer tube (20) communicate with reactor (1).Be put in lower to level ball (21), continue to keep reactor (1) interior gas inlet tracheae (20).Reactor (1) from add liquid to be measured pick up counting the reaction 30min～60min stop the reaction.Open first charge pipe (2) and second charge pipe (3) respectively, the interior liquid of first charge pipe (2) and second charge pipe (3) is got in the reactor (1).After catching up with the interior gas of most reactor (1), turn eudiometer tube cock (19), closing capacity tracheae (20).Open reactor leakage fluid dram (11) tongs, make waste reaction solution all flow into returnable bottle (33).Mention level ball (21), turn eudiometer tube cock (19) is all caught up with gas into gas washing hemisphere (27).Turn eudiometer tube cock (19), closing capacity tracheae (20).Open the stirring rate of the interior magneton of big gas washing hemisphere (27) (29), keep 2～5min.The stop magnetic agitation (30) of gas washing hemisphere (27), cock on the turn eudiometer tube (19) reduces level ball (21); Catch up with the interior gas of gas washing hemisphere (27) into eudiometer tube (20); When gas washing flow to eudiometer tube cock (19) when locating, turn eudiometer tube cock (19), closing capacity tracheae (20).Improve level ball (21), make interior liquid levels of level ball (21) and the interior liquid surface level of eudiometer tube (20), read eudiometer tube (20) scale, recording volume V, record air pressure this moment and temperature are calculated after being used for simultaneously.
The present invention compares original technology and has following advantage:
1, reaction does not receive the external environmental condition variable effect, compares the normal form amino acid determining instrument and can measure under the low temperature in winter.Determination data is stable, and average error reduces half the than the normal form amino acid determining instrument.
2, can the conditioned reaction temperature through circulator bath, sense cycle is short, and the reaction time shortens 1/3 than the normal form amino acid determining instrument.
3, gas washing hemisphere (27) is furnished with magnetic agitation (10), gas washing automatically.Reactor (1) is furnished with magnetic agitation (30), can react fully and carry out, the conditioned reaction process.
4, convenience for washing is cleaned respectively behind each part detachable, and reactor (1) and gas washing hemisphere (27) all can carry out self-cleaning through the magnetic agitation (10) of reactor (1) and the stirrer (30) of gas washing hemisphere (27).
5, the adding of recovery section (IV) makes course of reaction cleaner; Waste reaction solution (mixed liquor of sodium nitrite, glacial acetic acid and liquid to be measured) and gas washing waste liquid (potassium permanganate, NaOH mixed liquor) can directly enter returnable bottle through silicone tube (32); And self-cleaning can react to each other between the waste liquid; Reaction produces waste gas and all discharges through recovery section (IV) is unified, keeps clean environment.
6, volume is little, is convenient to place, and except that retracting device (IV), all can be positioned on the experiment table and operate.
Description of drawings:
Fig. 1 primary amino radical analyzer of the present invention synoptic diagram.Wherein:
1; Reactor 2; First charge pipe 3; Second charge pipe 4; Water-bath chuck 5; Reactor wall 6; Circulator bath interface 7; The first thin neck feed pipe 8; The second thin neck feed pipe 9; Magneton 10; Magnetic agitation 11; Discharging tube 12; Reactor ground 13; Grinding port plug 14; Three-limb tube 15; Three-way cock 16; Gas outlet 17; Thin neck bend pipe 18; Thin neck straight tube 19; Inclined hole stop,threeway 20; Eudiometer tube 21; Level ball 22; Emulsion tube 23; Thin neck connecting pipe 24; Thin neck separator tube 25; Discharging tube 26; Buffering ball 27; Gas washing hemisphere 28; Feed tube 29; Magneton 30; Magnetic agitation 31; Four-way connecting pipe 32; Silicone tube 33; Returnable bottle 34; Feed tube 35; Gas outlet 36; Plug
Specific embodiments:
Following examples are to further specify of the present invention, but the present invention is not limited thereto.
Embodiment 1
Primary amino radical acidity test appearance according to the invention is made up of reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV).
Preferably, reaction unit (I) comprises reactor (1), first charge pipe (2), second charge pipe (3) and three-limb tube (14).Wherein reactor contains water-bath chuck (4), contains two interfaces (6) on water-bath chuck (4) outer wall, is used to connect circulator bath.Preferably, reactor bottom is flat, contains the first thin neck glass tube (7), the second thin neck glass tube (8) and a downward drainage conduit (11).Wherein first thin neck glass tube (7) one ends connect first charge pipe (2), and the other end passes water-bath chuck (4) and connects with reactor wall (5), is used for the adding of reactant liquor; Second thin neck glass tube (8) one ends connect second charge pipe (3), and the other end passes water-bath chuck (4) and connects with reactor wall (5), is used for the adding of liquid to be measured; Drainage conduit (11) is passed water-bath chuck (4) and is connected with reactor wall (5), is used for the discharge of reactor (1).Drainage conduit (11) is connected with four-way connecting pipe (31) in the retracting device (IV) through silicone tube, and drainage conduit (11) is furnished with tongs.Preferably, reactor (1) contains magneton (9), the supporting magnetic agitation in bottom (10).Reactor (1) top is ground (12), links to each other with the ground piston of three-limb tube.Three-limb tube (14) institute band glass tube is thin neck glass tube, and intersection is three hole cocks (15).An end (13) of band grinding port plug is connected with reactor ground (12) in three ends of three-limb tube; One end of exhausr port (16) is connected with four-way connecting pipe (31) in the retracting device (IV) through silicone tube, and last end passes through thin neck bend pipe (17) and links to each other with inclined hole stop,threeway (19).
Preferably, amount device of air (II) comprises eudiometer tube (20) and level ball (21).Wherein inclined hole three-way cock (19) is contained in the eudiometer tube upper end, and the cock upper end is two thin neck glass tubes; Wherein bend pipe (17) connects three-limb tube, and thin neck straight tube (18) is connected with gas washing hemisphere (27) through the thin neck connecting pipe (23) in the air-washer (III).Preferably, venturi portion is amount gas part, scale range 10～15ml, minimum scale 0.05ml in the eudiometer tube; The eudiometer tube bottom is gas buffer part (effect is to prevent that gas from too much causing gas to overflow from level ball (21)), and the buffer portion volume is about 150～200ml, and interface is contained in the bottom, is connected with level ball (21) through emulsion tube.Preferably, the level sphere volume is about 200～250ml, is positioned over lower.
Preferably, air-washer (III) comprises thin neck connecting pipe (23), gas washing hemisphere (27) and buffering ball (26).Wherein thin neck connecting pipe one end is connected with eudiometer tube (20) through thin neck straight tube (18), and the other end is connected with gas washing hemisphere (27) through separator tube (24).Preferably, gas washing hemisphere (27) is flat, and radius is about 100～150mm, includes magneton (29), supporting magnetic stirring apparatus (30).Two glass tubes are contained in gas washing hemisphere bottom, and wherein downward-sloping is discharging tube (25), is used for the discharging of gas washing liquid, are connected with four-way connecting pipe (31) in the retracting device (IV) through silicone tube; 90 ° of make progress bend pipe (28) and buffering ball (26) lower ends.Preferably, buffering ball (26) radius is about 80～120mm, and top is the funnel-form inlet, and bore is about 50～70mm, is convenient to the adding of gas washing liquid.
Preferably, retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33).Wherein three interfaces of four-way connecting pipe (31) one ends connect exhausr port (16), reactor leakage fluid dram (11) and gas washing hemisphere leakage fluid dram (25) respectively, and the interface of the other end is connected with feed tube (34) through silicone tube.Preferably, returnable bottle (33) volume is 10-20L, is used for the recovery of waste reaction solution and deposits; Returnable bottle (33) is suitable for reading is furnished with plug (36), contains feed pipe (34) and escape pipe (35) on the plug, and escape pipe (35) is directly connected in hood or the fuming cupboard gas outlet through silicone tube, prevents gas dissipation.
Primary amino radical acidity test appearance according to the invention, its reaction unit (I), amount device of air (II), air-washer (III) can be positioned on the experiment table, get final product with iron stand is fixing.Retracting device (IV) is positioned over the place that horizontal level is lower than reaction unit (I) and air-washer (III), and handles at any time.
Embodiment 2
1. experiment is prepared:
Carry out preliminary work during use of the present invention earlier; At first to prepare gas washing liquid (potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400m1); Smeared vacuum grease to each piston then; Reactor (12) suitable for reading twines and seals film and fix with clip, and reactor discharging tube (11) and gas washing hemisphere discharging tube (25) clip with tongs, and reactor jacket (4) communicates with circulator bath.Three-limb tube cock (15) revolve
eudiometer tube cock (19) revolve " " (like eudiometer tube cock (19) among the figure one), guaranteed discharge tracheae (20) communicates with retracting device (IV) through three-limb tube gas outlet (11).Inject deionized water from level ball (21); Improve level ball (21) (being higher than eudiometer tube cock (19)); Drive gas out of from three-limb tube gas outlet (11), eudiometer tube (20) is filled with deionized water after, (19) 90 ° of turn eudiometer tube cocks become horizontal direction; Closing capacity tracheae (20), maintenance dose tracheae (20) is full of water state.Pour gas washing liquid into half bottle of gas washing (27) from surge flask (26) at last; Cock on the turn eudiometer tube (19) becomes " // "; Maintenance dose tracheae (20) communicates with gas washing hemisphere (27); Reduce level ball (21), gas washing hemisphere (27) interior gas soakage tracheae (20), when gas washing flow to eudiometer tube cock (19) when locating (assurance leakage fluid dram (25) locates not deposit gas).(19) 180 ° of one-tenth of turn eudiometer tube cock " ", make eudiometer tube (20) and gas washing hemisphere (27) closure, and communicate with three-limb tube (14).Improve level ball (21); Drive gas out of from three-limb tube gas outlet (11); Eudiometer tube (20) is filled with deionized water (three-way pipe (14) link to each other with eudiometer tube (20) thin neck in no gas residue), and turn eudiometer tube cock (19) is to horizontal direction, closing capacity tracheae (20).(15) 180 ° of one-tenth of turn three-limb tube cock
reactor (1) communicates with retracting device (IV) through three-limb tube gas outlet (11).Be put in lower to level ball (21), equal full of liquid in gas washing hemisphere this moment (27) and the eudiometer tube (20), and and isolate from outer air.Open circulator bath and magnetic agitation (10) (in the level experiment, circulator bath temperature constant, reactor (1) lower magnetic force stirring (10) invariablenes turning speed).
2. specimen:
Add the about 20～30ml of glacial acetic acid from first charge pipe (2) earlier during test sample of the present invention; Then add 40% the about 20～30ml of sodium nitrite in aqueous solution (the interior liquid of reactor (1) reaches reactor more than 3/4); Turn first charge pipe (2) and second charge pipe (3) cock; Make first charge pipe (2) and second charge pipe (3) closure, reactor (1) only links to each other with retracting device (IV) through three-limb tube gas outlet (11).Reactor (1) internal reaction generates NO or NO
2Gas keeps more than 2～5min, guarantees all to discharge the interior air of reactor (1).Turn three-limb tube cock (15) becomes
makes reactor (1) sealing, and eudiometer tube (20) does not communicate with the external world yet simultaneously.Turn first charge pipe (2) and second charge pipe (3) cock; First charge pipe (2) and second charge pipe (3) are opened; Producing gas in the reactor (1) drives liquid out of from first charge pipe (2) and second charge pipe (3); After gas was driven out of fully in the thin neck of first charge pipe (2) and second charge pipe (3) bottom, turn first charge pipe (2) and second charge pipe (3) cock made first charge pipe (2) and second charge pipe (3) closure.Turn eudiometer tube cock cock (19) one-tenth " ", reactor (1) is only communicated with eudiometer tube (20), be hedged off from the outer world, (reactor this moment (1) is merely NO or the NO that reacts generation with the interior gas of eudiometer tube (20) to keep reactor (1) interior gas inlet tracheae (20)
2Gas).In charge pipe (2), add deionized water (account for volume 3/4, play the fluid-tight effect, prepare for the experiment back simultaneously).In second charge pipe (3), add testing protein solution (like needs; Please heat the maintenance protein solution is working fluid), slowly open second charge pipe (3) cock, make liquid to be measured slowly get into reactor (1) and (do not add; Stay trace, prevent that air from getting into reactor (1)).Closed second charge pipe (3) cock is washed second charge pipe (3) (5ml～10ml), add about 1～2ml n-amyl alcohol (n-amyl alcohol and solution layering again with small amount of deionized water; Be in the solution top), slowly open second charge pipe (3) cock, make solution slowly get into reactor (1); Closed cock when n-amyl alcohol arrives second charge pipe (3) cock place; Add deionized water (account for volume 3/4, play the fluid-tight effect, prepare for the experiment back simultaneously).In the course of reaction; When gas in the eudiometer tube (20) surpasses the eudiometer tube venturi portion; Improve level ball (21) rapidly, the cock of turn eudiometer tube becomes " // " for (19) 180 °, and maintenance dose tracheae (20) communicates with gas washing hemisphere (27); Catch up with gas into gas washing hemisphere (27) and (to open the magnetic agitation (9) below the gas washing hemisphere (27), to make NO and NO
2Gas is absorbed by gas washing liquid rapidly); After gas in the eudiometer tube (20) is caught up with only; (19) 180 ° of one-tenth of turn eudiometer tube cock " ", make eudiometer tube (20) and gas washing hemisphere (27) closure, and communicate with reactor (1); Be put in lower to level ball (21), continue to keep reactor (10) interior gas inlet tracheae (20).Reactor (1) from add liquid to be measured pick up counting the reaction 30～60min (the process domestic demand is repeatedly caught up with gas into gas washing hemisphere (27)), stop the reaction.Open first charge pipe (2) and second charge pipe (3) cock respectively; The interior liquid of first charge pipe (2) and second charge pipe (3) is got in the reactor (1); Catch up with air in the thin neck of first charge pipe (2) and second charge pipe (3) bottom in the reactor (1); Closed second charge pipe (3) cock keeps first charge pipe (2) cock to open.Along with liquid continuous adding, the interior gas of reactor (1) is all caught up with into eudiometer tube (20).When liquid is arrived in three-limb tube cock (15) when locating, the cock of turn eudiometer tube becomes horizontal direction for (19) 90 °, closing capacity tracheae (20), closed first charge pipe (2) cock simultaneously.Turn three-limb tube cock (15) becomes
opens reactor leakage fluid dram (11) tongs, makes waste reaction solution all flow into returnable bottle (33).Close tongs; Open first charge pipe (2) cock; Add deionized water to reactor (1) and be full of, closed first charge pipe (2) cock is with the automatic cleaning reaction device (1) (unlatching that keeps reactor (1) circulator bath and magnetic agitation (10) in the course of reaction) of magnetic agitation (10).Mention level ball (21), turn eudiometer tube cock (19) becomes " // ", all catches up with gas into gas washing hemisphere (27) (the no gas residue of narrower neck tube (24) above the gas washing hemisphere (27)), and the cock of turn eudiometer tube becomes horizontal direction, closing capacity tracheae (20) for (19) 90 °.Open the stirring rate of the interior magneton of big gas washing hemisphere (27) (29), keep 2～5min.The stop magnetic agitation (30) of gas washing hemisphere (27); Cock on the turn eudiometer tube (19) becomes " // ", and maintenance dose tracheae (20) communicates with gas washing hemisphere (27), reduces level ball (21); Gas washing hemisphere (27) interior gas soakage tracheae (20); When gas washing flow to eudiometer tube cock (19) when locating, the cock of turn eudiometer tube becomes horizontal direction, closing capacity tracheae (20) for (19) 90 °.Improve level ball (21), make interior liquid levels of level ball (21) and the interior liquid surface level of eudiometer tube (20), read eudiometer tube (20) scale, recording volume V, record air pressure this moment and temperature are calculated after being used for simultaneously.
3. experiment aftertreatment:
Turn eudiometer tube cock (19) one-tenth " ", turn three-limb tube cock (15) becomes
maintenance dose tracheae (20) to link to each other with retracting device (IV) through three-limb tube gas outlet (16).Mention level ball (21); Drive gas out of from three-limb tube gas outlet (16); Eudiometer tube (20) is filled with deionized water; The cock of turn eudiometer tube becomes horizontal direction for (19) 90 °, and closing capacity tracheae (20), maintenance dose tracheae (20) are full of water state (the interior no gas residue of thin neck glass tube between three-way cock (15) and the inclined hole three-way cock (19)).Turn three-limb tube cock (19) becomes
makes eudiometer tube (20) and three-limb tube (14) closure, and reactor (1) communicates with retracting device (IV) through three-limb tube gas outlet (16).Be put in lower to level ball (21), open reactor leakage fluid dram (11) tongs, the interior liquid of emptying reactor (1) is closed leakage fluid dram (11) tongs, prepares the next test of treating test sample.In the test sample process, gas washing liquid is become when dark blue by dark purple, opens leakage fluid dram (25) tongs, emptying gas washing hemisphere (27) liquid.Close leakage fluid dram (25) tongs, add new gas washing liquid again.After test reaction is all intact, open reactor leakage fluid dram (11) and gas washing hemisphere leakage fluid dram (25) tongs, emptying reactor (1) and the interior waste liquid of gas washing hemisphere (27).Add in glacial acetic acid and sodium nitrite mixed liquor to the gas washing hemisphere (27) from buffering ball (26), open the interior magneton of big gas washing hemisphere (27) (29) rotating speed, the gas washing liquid of washing off on gas washing hemisphere (27) inwall is residual.Again after the effluent discharge, with washed with de-ionized water one time.Be potassium permanganate, NaOH, glacial acetic acid and the sodium nitrite mixed liquor that reactor (1) and gas washing hemisphere (27) are discharged in the retracting device (IV), self-absorption reacts to each other.The NO and the NO that produce
2Gas is handled by unified discharge of exhausr port (35).As treat that test sample is prone to produce great amount of bubbles, and add preceding need of liquid to be measured and in reactor (1), add a small amount of n-amyl alcohol, be used for froth breaking.
4. calculate
Following formula has provided the computing formula of primary amino radical analyzer and the setting method of related parameter has been arranged.
Note n
AppearanceBe sample primary amino radical molar weight, n
N2By being surveyed the nitrogen molar weight, can know that by reaction principle the mol ratio of primary amino radical reaction generation nitrogen is 1: 1, then this equation can be expressed as:
n
Appearance=n
N2(1)
Note c is sample molar content (mol/g), and m is sample quality (m), and then equation can be expressed as:
n
Appearance=cm (2)
Note ρ is the mass density (g/ml) of nitrogen, and tabling look-up according to ambient temperature and the atmospheric pressure of amount during gas obtains, and V is for measuring the volume (ml) of nitrogen, M be nitrogen molecule amount (mol/g) then equation can be expressed as:
n
N2＝ρV/M (3)
Bring formula (2), (3) in (1) into, and arrangement obtains:
Can calculate the primary amino radical content of sample through formula (4).
Claims (9)
1. primary amino radical analyzer; Form by reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV); It is characterized in that; Reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV) connect successively, and the exhausr port and the leakage fluid dram of reaction unit (I), amount device of air (II), air-washer (III) all are connected on the recovery section (IV).
2. primary amino radical analyzer as claimed in claim 1 is characterized in that, described reaction unit (I) comprises reactor (1), charge pipe (2) and three-limb tube (14); Three-limb tube (14) has cock (15), and cock (15) is positioned at three-limb tube (14) intersection, is used for the trend of adjustments of gas in three-limb tube (14).
3. primary amino radical analyzer as claimed in claim 2 is characterized in that, described reactor (1) top is ground (12), and the bottom is flat, has water-bath chuck (4); A thin neck glass tube (7) and a downward drainage conduit (11) upwards arranged at reactor (1) bottom; One end of thin neck glass tube (7) connects charge pipe (2), and the other end passes chuck (4) and connects with reactor wall (5); Drainage conduit (11) is passed chuck (4) and is connected with reactor wall (5), is used for the discharge of reactor (1); Contain two interfaces (6) on reactor jacket (4) outer wall, be used for the communication loop water-bath; Reactor (1) contains magneton (9), the supporting magnetic agitation in bottom (10).
4. primary amino radical analyzer as claimed in claim 3 is characterized in that, described reaction unit (I) comprises two charge pipes---first charge pipe (2) and second charge pipe (3); First charge pipe (2) and second charge pipe (3) bottom are thin neck glass tube, and first charge pipe (2) is 25～35ml, and second charge pipe (3) is about 10～20ml; Reaction unit (I) comprises two thin neck glass tubes, and the first thin neck glass tube (7) and the second thin neck glass tube (8) connect first charge pipe (2) and second charge pipe (3) respectively.
5. primary amino radical analyzer as claimed in claim 3; It is characterized in that; Three-limb tube (15) is connected with reactor top ground (12) through the grinding port plug (13) of thin neck glass tube one end, and the other end of three-limb tube (15) links to each other with inclined hole stop,threeway (19) through thin neck bend pipe (17).
6. primary amino radical analyzer as claimed in claim 1 is characterized in that, air-washer (III) comprises gas washing hemisphere (27) and buffering ball (26); Gas washing hemisphere (27) and buffering ball (26) are connected with inclined hole stop,threeway (19) through thin neck glass connecting pipe (23); Gas washing hemisphere (27) radius is 100～150mm, and buffering ball (26) radius is 80～100mm.
7. primary amino radical analyzer as claimed in claim 6 is characterized in that, gas washing hemisphere (27) top connects thin neck glass tube (24), is used for the gas turnover; The bottom has a downward glass tube (25) and is used for discharge opeing, and have one 90 ° upwards bend pipes (28) be used to connect buffering ball (26); Gas washing hemisphere (27) is flat, includes magneton (29), supporting magnetic stirring apparatus (30).
8. primary amino radical analyzer as claimed in claim 1 is characterized in that, described retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33).
9. like the method for application of each described uncle's ammonia quantitative instrument of claim 1～8, comprise the following steps:
1) preliminary work:
(potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400m1) fill with gas washing hemisphere (27) with gas washing liquid earlier.Again eudiometer tube (20) is filled with deionized water.And keep equal full of liquid in gas washing hemisphere (27) and the eudiometer tube (20), and and isolate from outer air.Open circulator bath and magnetic agitation (10);
2) test sample:
Add glacial acetic acid 20～30ml from first charge pipe (2) earlier, then add 40% the about 20～30ml of sodium nitrite in aqueous solution.Reactor (1) internal reaction generates NO or NO
2Gas, air in the emptying reactor 1.Drive gas in the thin neck of first charge pipe (2) and second charge pipe (3) bottom out of.Keep reactor (1) only to communicate through the adjustment cock with eudiometer tube 20, isolated with ambient atmosphere.In second charge pipe (3), add testing protein solution, with the n-amyl alcohol fluid-tight.Reaction 30～60min stops reaction.In eudiometer tube (20), catch up with the gas that produces into gas washing hemisphere (27).Catch up with the interior residual gas of gas washing hemisphere (27) into eudiometer tube (20) at last.Read eudiometer tube (20) scale, recording volume V, record air pressure this moment and temperature simultaneously.
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| CN201110249480.1A CN102393466B (en) | 2011-08-29 | 2011-08-29 | Primary amino radical tester |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110249480.1A CN102393466B (en) | 2011-08-29 | 2011-08-29 | Primary amino radical tester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794442A (en) * | 2012-07-23 | 2012-11-28 | 宁夏共享集团有限责任公司 | Liquid material device for preventing contact of liquid material and air to react for casting |
| CN103018077A (en) * | 2012-12-28 | 2013-04-03 | 河南师范大学 | Leakage detection sampler |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5528923A (en) * | 1992-12-21 | 1996-06-25 | Ledez; Kenneth M. | Gas amount and solubility investigation apparatus |
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2011
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5528923A (en) * | 1992-12-21 | 1996-06-25 | Ledez; Kenneth M. | Gas amount and solubility investigation apparatus |
Non-Patent Citations (4)
| Title |
|---|
| DONALD D. VAN SLYKE: "Manometric Determination of Primary Amino Nitrogen and its Application to Blood Analysis", 《JOURNAL OF BIOLOGICAL CHEMISTRY》, vol. 83, 31 December 1929 (1929-12-31) * |
| VAN SLYKE D D: "Eine Methode zur quantitativen Bestimmung der aliphatischen Aminogruppen; einige Anwendungen derselben in der Chemie der Proteine, des Harns und der Enzyme", 《BERICHTE DER DEUTSCHEN CHEMISCHEN GESELLSCHAFT》, 31 December 1910 (1910-12-31) * |
| 张志贤: "《实用有机定量分析》", 31 March 1965, article "实用有机定量分析" * |
| 郑燕龙，潘子昂: "《实验室玻璃仪器手册》", 31 May 2007, article "范氏氨基酸测定器" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102794442A (en) * | 2012-07-23 | 2012-11-28 | 宁夏共享集团有限责任公司 | Liquid material device for preventing contact of liquid material and air to react for casting |
| CN103018077A (en) * | 2012-12-28 | 2013-04-03 | 河南师范大学 | Leakage detection sampler |
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| CN102393466B (en) | 2014-10-08 |
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