CN101398387A - Preparation of am detection test paper for milk and solution and am detection method - Google Patents
Preparation of am detection test paper for milk and solution and am detection method Download PDFInfo
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- CN101398387A CN101398387A CNA2008102319800A CN200810231980A CN101398387A CN 101398387 A CN101398387 A CN 101398387A CN A2008102319800 A CNA2008102319800 A CN A2008102319800A CN 200810231980 A CN200810231980 A CN 200810231980A CN 101398387 A CN101398387 A CN 101398387A
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Abstract
The invention provides a preparation method of ammonium group detection test paper in milk and milk solution and a detection method of ammonium group; potassium iodide is taken and dissolved in water and mixed; during the stirring process, mercuric chloride (HgCl2) powder or mercuric iodide (HgI2) powder with small quantity is dripped in the potassium iodide solution by batch and sufficiently mixed; the dripping is stopped till that slight imperial red deposition HgI2 generated in the solution is not dissolved; subsequently, the solution is diluted by deioned water so as to obtain a dry reagent raw solution which is uniformly fixed on a testing carrier by the forms of coating, printing or soaking and dried so as to obtain the ammonium group detection test paper. The liquid to be detected or the water solution of the solid to be detected together with the developer are dripped on the test paper; and if the liquid to be detected contains ammonium group, the color of the ammonium group detection test paper changes to yellowish brown. Compared with the traditional ammonium group detection method, the detection method meets the requirements of simpleness, fastness and portableness; and simultaneously, the shelf life of the reagent is greatly prolonged.
Description
Technical field
The present invention relates to the fast qualitative or the half-quantitative detection of ammonium salt in food security, environment and the public health monitoring, be specifically related to the preparation of ammonium root detection test paper in a kind of breast and the solution and the detection method of ammonium root.
Prior art
It is the common project of environment department, public health department and food security supervision department that ammonium salt detects.Its laboratory detection method is many, but all is difficult to satisfy the requirement of current efficient supervision to its " easy, quick and portable ".
Just ammonium salt class such as ammonium sulfate, ammonium chloride etc. are the ammonium root that can dissociate after water-soluble.Therefore the detection of ammonium root becomes the foundation that this class material detects.The method of common mensuration ammonium salt has phynol method and nessler reagent (Nessler ' s Reagent) method etc., has also occurred the KI-NaClO development process in the recent period.Below analyze with regard to this several method:
1. phynol method: when this method detects ammonium root, require the water-bath heating to develop the color and complicated operation, be not suitable for on-the-spot the detection.
The paper of 2.KI-NaClO development process: Dong Wenbin etc. " ammonium salt fast detecting Study of New Method in the fresh milk ", China's dairy industry, 2004,32 (8): the 35-37 page or leaf, with the KI-NaClO development process that Chinese patent 200410026304.1 is addressed, the defective of following aspect is arranged:
1) the independent detection reagent KI and the NaClO that use of this method is improper.Because the KI solid " easy deliquescence in soft air is met light and air and can be separated out free-iodine and be yellow ", " aqueous solution is met the light flavescence, and separates out free-iodine " of potassium iodide.As seen no matter be liquid or solid, the preservation of KI all is the requirement specific condition.Address " consider the preservation of long-term use to KI, KI adds with solid dosage form " in the former paper, 200410026304.1 also address and will at first potassium iodide be processed into tablet.But these improvement are also failed fundamentally to solve it and are met the wet problem of separating out elemental iodine and being difficult to preserve.
About NaClO, point out in the chemical industry dictionary that sodium hypochlorite is " extremely unstable solid, its aqueous solution react acid can be decomposed into sodium chloride, sodium chlorate and oxygen gradually, are strong oxidizers ", as seen, no matter solid or liquid, the active principle ClO that detectable needs
-In storage, all can reduce gradually; Former paper is also pointed out this reagent, and " NaClO concentration can not be too rare, considers the prolongation to the storage life of solution, and the dilution ratio of NaClO is to be advisable greater than 1/4." Given this, the more impossible exploitation afterwards of this reagent becomes convenient and practical dried reagent product.
2) this detection method needs the professional could guarantee testing result, and is too strict because operation skill requires, and is not suitable for promoting.We find when repeating its experiment, need careful during operation, can not rock test tube, otherwise do not observe phenomenon or phenomenon is not obvious, former paper also emphasizes " solution joins in the milk sample to be checked slowly with transfer pipet, notes not disturbance contact interface layer ", and when adding solution " speed should slow down as far as possible; and should not shake color comparison tube, be beneficial to observe change color.”
3) detect strict reagent and add order, the operator is careless slightly to add in reverse order words with reagent, will cause the appearance of false negative result.Detect and require to add earlier KI solution, add the mixed liquor of NaClO and NaOH again.Former paper is described: " after the mixed liquor that adds NaClO and NaOH earlier shakes up, add KI solution again, reagent contact interface and present orange redly with the upper part thinks it mainly is to produce free I by analysis if conversely
2Cause, and peculiar black does not appear." but black is only the color that manifest here.
4) last, the apparent color fugitive color of this method is led the carelessness in the testing process easily or is offed normal temporarily and cause judging by accident.Original text is pointed out " because the color instability that presents along with time lengthening can be faded, is good so see chromatic effect within 1 minute after adding reagent." visible its invention reagent and being not suitable for as the field test method.
3. nessler reagent colourimetry: this method is to measure the national standard method of ammonia-nitrogen content in water body and the air, and the effective constituent of detectable is closed mercury ion [HgI for the tetraiodo of alkalescence
4]
2-, advantage is its detection sensitivity height, chance ammonium or ammonia colour developing present bright-coloured yellowish-brown and are easy to distinguish.But this reagent has 2 aspect shortcomings, on the one hand in preservation since its to the continuous absorption generation color reaction of ammonia in the air and gradually desensitising finally lose effectiveness, therefore need positive confinement and low temperature keeping reagent or matching while using, very inconvenience.Second aspect contains mercury salt in this reagent, and the conventional reagents consumption brings certain pollution threat to environment, therefore need reduce consumption as far as possible.
More than several ammonium salt monitoring methods such-and-such defective is all arranged, the field test that can't realize easily and fast, be suitable for.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide that the ammonium root detects the preparation of test paper and the detection method of ammonium root in a kind of easy, fast qualitative or half-quantitative detection breast and the solution.
For achieving the above object, the preparation method that ammonium root of the present invention detects test paper is: it is soluble in water 1) at first to get potassium iodide, stirs down mercuric chloride (HgCl
2) the powder gradation joins in the liquor kalii iodide on a small quantity, fully stirs mixedly, when solution micro-vermilion precipitation occurs and no longer dissolves, stops to drip, and adds deionized water, the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste; Or stir down mercuric iodixde (HgI
2) powder repeatedly is incorporated in the liquor kalii iodide on a small quantity, fully stirs mixedly, micro-vermilion precipitation occurs up to solution and stops when no longer dissolving, and gets supernatant, adds deionized water, the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste;
2) but dried reagent stoste evenly be fixed on not on quantitative filter paper, qualitative filter paper or the chromatography filter paper test carrier in the water absorptivity solid phase material with dried reagent stoste generation chemical reaction and be drying to obtain the ammonium root by coating, printing or the mode of soaking detect test paper.
The method that the present invention detects ammonium root in breast and the solution is:
1) at first detects test paper and dip in the aqueous solution of getting liquid to be checked or solids to be checked, again to dripping a drop of liquid developer on it with the ammonium root; Perhaps dip in ammonium root detection test paper earlier and get chromogenic reagent solution, drip a liquid to be detected again; Perhaps detect test paper with root and dip in the equal-volume premixed liquid of getting liquid to be checked and developer, said developer is the OH that contains 1-5mol/L
-NaOH or the deionized water solution of KOH;
2) in the described liquid to be checked if contain the ammonium root, the ammonium root detects the test paper variable color becomes yellowish-brown, color depth and ammonium radical content are proportionate, and according to shade, contrast the semiquantitative determination that just can carry out the ammonium root with colorimetric card; Described colorimetric card is that the ammonium root detects one group of photochrome or the picture that test paper formed color in the ammonium root solution of normal concentration presents graded.
The present invention compares with traditional ammonium root detection method has following characteristics:
1. easily and fast, portable
Only need test paper and developer when the present invention detects, volume is convenient for carrying for a short time; When using, developer can extrude one, just the complicated quantitatively equipment of alternative laboratory operation as dripping eyedrop; It is quick rapidly to detect the result, reacts on moment to carry out, and colour developing fully only needs 10-30 second, and is bright-colored, is convenient to distinguish feminine gender or positive findings, easy to use.Satisfy market to its " simple, quick, portable " requirement.
2. keep the advantage of National Standard Method, but solved the problem of its existence
Compare with GB nessler reagent detection method, the present invention is outside keeping its high sensitive and the bright-coloured advantage of colour developing, on the one hand by preparing test paper and developer respectively, make the Preservation of Reagent problem be resolved, in September, 2008, we test the mummification test paper that make in July, 2006, find that it is still effective, and this test paper storage life at least 2 years are described.Thereby make this test paper walk out laboratory performance effect more widely.On the other hand, the present invention detects and to be micromanipulation, consumes reagent few (every sample detects and only consumes mercury salt solution 10ul), reduces by 2 orders of magnitude than the Routine Test Lab operation, has significantly reduced environmental pollution and reduces cost;
Strong to covering, insensitive ammonium salt that develops the color is mingled cow's milk and is detected, and its ammonium root detects least concentration and is not higher than 20mg/100mL.The aqueous solution good to transparency, its ammonium root detect least concentration and are not higher than 5mg/100mL.
3. application face width.All materials that contains the ammonium root all can this method detect.Can offer environment, public health and food security supervision department are used for the examination of object in violation of rules and regulations; Also can promote into family, satisfy voluntarily detection and the strick precaution of people environment especially food security; Or other industry is used for qualitative or half-quantitative detection ammonium root.
Description of drawings
Fig. 1 is that simulation ammonium sulfate is mingled newborn testing result photo;
Fig. 2 is that simulation ammonium chloride is mingled newborn testing result photo;
Fig. 3 is that simulation ammonium nitrate is mingled newborn testing result photo;
Fig. 4 is a variable concentrations ammonium sulfate tap water testing result photo;
Fig. 5 is a variable concentrations ammonium chloride tap water testing result photo;
Fig. 6 is a variable concentrations ammonium nitrate tap water testing result photo.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
One, the ammonium root detects the preparation of test paper:
1) the dried reagent stoste of preparation: 2 kinds of compound methods are arranged, as follows
Method one: it is soluble in water to get potassium iodide, stirs down mercuric chloride (HgCl
2) the powder gradation joins in the liquor kalii iodide on a small quantity, fully stirs mixedly, when solution micro-vermilion precipitation occurs and no longer dissolves, stops to drip, and adds deionized water, the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste;
Method two: it is soluble in water to get potassium iodide, stirs down mercuric iodixde (HgI
2) powder repeatedly is incorporated in the liquor kalii iodide on a small quantity, fully stirs mixedly, micro-vermilion HgI occurs up to solution
2Precipitation stops when no longer dissolving, and gets supernatant, adds deionized water, and the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste;
2) the ammonium root detects the preparation of test paper
Dried reagent stoste evenly is fixed on the test carrier and is drying to obtain the ammonium root by coating, printing or the mode of soaking detect test paper.But carrier be not with the water absorptivity solid phase material such as the quantitative filter paper of dried reagent stoste generation chemical reaction, qualitative filter paper, chromatography filter paper etc.The ammonium root is detected test paper be cut into suitable shape and size on demand, be connected on hand and hold on the handle and use.
Two, liquid developer preparation:
NaOH or KOH are dissolved in the OH that obtains containing 1-5mol/L in the deionization
-Deionized water solution.
Three, the making of colorimetric card
Detect the ammonium root solution fresh certified milk preparation of detection paper and the normal concentration tap water preparation with the ammonium root respectively, note and detect photochrome or the picture that formed color presents graded, respectively the colorimetric card that detects as ammonium salt in ammonium salt detection in the dairy products and the general aqueous solution.
Four, detect the method for ammonium root in breast and the solution
When detecting at the scene, if thing to be checked is that solution then directly detects according to following step; When if thing to be checked is solid (as milk powder, soil etc.), then will detect by the following step again behind the solid thing wiring solution-forming to be checked.
Detection method has 3 kinds, and different reagent adding methods does not influence testing result.
Detection method one
1) detecting test paper with the ammonium root dips in to get liquid to be checked or drip liquid to be checked and makes its suction infiltration.
2) to dripping one of developer on the test paper that soaks into;
3) observe: if contain the ammonium root, will make the test paper variable color become yellowish-brown in the liquid to be checked, color depth and ammonium radical content positive correlation with the colorimetric card contrast, just can be learnt ammonium root concentration range in the solution.
Detection method two:
1) gets the ammonium root and detect test paper, drip one of developer thereon and make its infiltration;
2) get liquid to be checked, dropping one drops in to soak into to be had on the test paper of developer;
3) observe: with detection method one.
Detection method three:
1) gets liquid to be checked and the developer equal-volume is mixed into premixed liquid.
2) detecting test paper with the ammonium root dips in and gets premixed liquid or to 2 of dropping premixed liquids it on;
3) observe: with detection method one.
The principles of chemistry that the present invention relates to
In the dried reagent stoste process for preparation, be in liquor kalii iodide, slowly to add mercuric chloride (perhaps mercuric iodixde), till micro-red precipitate occurs.During this time, potassium iodide and mercuric chloride react in aqueous solution and generate mercuric iodixde red precipitate (if directly substitute mercuric chloride with mercuric iodixde, just can omit this step reaction); When potassium iodide was excessive, mercuric iodixde and potassium iodide further reacted and generate the good flaxen potassium tetraiodomercurate K of solubility property
2[HgI
4].When potassium iodide has been consumed, HgI
2↓ no longer dissolved.Its reaction equation suc as formula 1 to formula 3.
2KI+HgCl
2＝HgI
2↓+2KCl (1)
HgI
2+2KI＝K
2[HgI
4] (2)
Above overall reaction: 4KI+HgCl
2=2KCl+K
2[HgI
4] (3)
The tetraiodo is closed mercury acid group ([HgI
4]
2-) for the iodine of soft acid soft base composition closes hydrargyrum complex, have good stability, therefore the potassium tetraiodomercurate of reaction generation can long-term stability be present on the test paper carrier.
When potassium tetraiodomercurate on the test paper runs into the ammonium root in alkaline aqueous solution, just react to generate mercuric iodixde ammonium (OHg
2NH
2I) yellowish-brown precipitation, thus can make test paper present color, and reaction equation is seen formula 4.
2K
2[HgI
4]+NH
4 ++4OH
-＝OHg
2NH
2I↓+7KI+3H
2O (4)
(yellowish-brown)
The present invention is with a kind of stable component (OH in traditional nessler reagent
-) as the packing of liquid reagent independence, another active principle [HgI
4]
2-Be combined in advance and make ammonium root detection test paper on the test paper, reached the purpose of reagent long preservation.We tested the ammonium root detection test paper of in July, 2006 preparation in September, 2008, and test findings proves that it is still effective.Therefore, the storage life of this reagent was at least 2 years.
When detecting at the scene, only need trace liquid to be checked and developer together are added on the dried reagent test strip (in proper order, inverted order or mix the back add all can), if contain the ammonium root in the liquid to be checked, chromogenic reaction will take place, therefore near detection is rolled off the production line color depth can realize the sxemiquantitative of ammonium root with ammonium radical content positive correlation.Chromogenic reaction moment carries out, and colour developing only needs 10-20 second fully.Keeping the highly sensitive while of nessler reagent like this, making to detect to become directly perceived fast simple, micro-environmental protection and saving, the pot-life of reagent also prolongs greatly simultaneously.
The applicant has prepared variable concentrations and different types of standard ammonium salt solution with cow's milk and tap water respectively, detects test paper with ammonium root of the present invention it is detected, and the result has been taken photo, is reported as follows:
Example 1
1. buy the pure cow's milk of brand, preparation contains the cow's milk of mingling of variable concentrations ammonium sulfate, and is to be checked.
2. get ammonium root of the present invention and detect test paper number, dip in respectively with glass rod and to get variable concentrations ammonium sulfate and mingle cow's milk, spread upon respectively on each test paper, on each test paper, drip one of developer more respectively, observe, within second moment to 10, variable concentrations ammonium sulfate is mingled the yellowish-brown that cow's milk presents different depth, the colour developing result as shown in Figure 1, digitized representation simulation is mingled the Ruzhong and is contained the amount of ammonium root (g/100mL) among the figure.
Example 2
1. buy the pure cow's milk of brand, preparation contains the cow's milk of mingling of variable concentrations ammonium chloride, and is to be checked.
2. get ammonium root of the present invention and detect test paper number, directly dip in respectively and get variable concentrations ammonium chloride and mingle the wetting test paper of cow's milk, on each test paper, drip observation of developer more respectively, within second moment to 10, variable concentrations ammonium chloride is mingled the yellowish-brown that cow's milk presents different depth, the colour developing result as shown in Figure 2, digitized representation simulation is mingled the Ruzhong and is contained the amount of ammonium root (g/100mL) among the figure.
Example 3
1, buy the pure cow's milk of brand, preparation contains the cow's milk of mingling of variable concentrations ammonium nitrate, and is to be checked.
2, get ammonium root of the present invention and detect test paper number, drip variable concentrations ammonium nitrate respectively thereon and mingle cow's milk, each developer is observed again, within second moment to 10, variable concentrations ammonium nitrate is mingled the yellowish-brown that cow's milk presents different depth, the colour developing result as shown in Figure 3, digitized representation simulation is mingled the Ruzhong and is contained the amount of ammonium root (g/100mL) among the figure.
Example 4
1, the polymer solution in water of preparation variable concentrations ammonium sulfate is to be checked.
2, get ammonium root of the present invention and detect test paper number, drip variable concentrations ammonium sulfate polymer solution in water respectively thereon, respectively drip observation of developer again, within second moment to 10, variable concentrations ammonium sulfate polymer solution in water presents the yellowish-brown of different depth, and the colour developing result as shown in Figure 4.
Example 5
1, the polymer solution in water of preparation variable concentrations ammonium sulfate is to be checked.
2, get ammonium root of the present invention and detect test paper number, dip in respectively with glass rod and to get variable concentrations ammonium chloride polymer solution in water, spread upon respectively on each test paper and make it moistening, on each test paper, drip observation of developer more respectively, within second moment to 10, variable concentrations ammonium chloride polymer solution in water presents the yellowish-brown of different depth, and the colour developing result as shown in Figure 5.
Example 6
The polymer solution in water of preparation variable concentrations ammonium nitrate, to be checked.
Get ammonium root of the present invention and detect test paper number, directly dip in respectively and get the wetting test paper of variable concentrations ammonium nitrate polymer solution in water, dripping developer on each test paper respectively observes, within second moment to 10, variable concentrations ammonium nitrate polymer solution in water presents the yellowish-brown of different depth, and the colour developing result as shown in Figure 6.
Claims (4)
1, the preparation method of ammonium root detection test paper in breast and the solution is characterized in that:
1) it is soluble in water at first to get potassium iodide, stirs down mercuric chloride (HgCl
2) the powder gradation joins in the liquor kalii iodide on a small quantity, fully stirs mixedly, when solution micro-vermilion precipitation occurs and no longer dissolves, stops to drip, and adds deionized water, the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste; Or stir down mercuric iodixde (HgI
2) powder repeatedly is incorporated in the liquor kalii iodide on a small quantity, fully stirs mixedly, micro-vermilion precipitation occurs up to solution and stops when no longer dissolving, and gets supernatant, adds deionized water, the mass concentration that makes potassium iodide is that 5-30% obtains dried reagent stoste;
2) dried reagent stoste evenly is fixed on the test carrier and is drying to obtain the ammonium root by coating, printing or the mode of soaking detect test paper.
2, the ammonium root detects the preparation method of test paper in breast according to claim 1 and the solution, it is characterized in that: but said carrier for not with the water absorptivity solid phase material of dried reagent stoste generation chemical reaction in quantitative filter paper, qualitative filter paper or chromatography filter paper.
3, the detection method of ammonium root in breast and the solution is characterized in that:
1) at first detects test paper and dip in the aqueous solution of getting liquid to be checked or solids to be checked, again to dripping a drop of liquid developer on it with the ammonium root; Perhaps dip in ammonium root detection test paper earlier and get chromogenic reagent solution, drip a liquid to be detected again; Perhaps detect test paper and dip in the equal-volume premixed liquid of getting liquid to be checked and developer with root;
2) in the described liquid to be checked if contain the ammonium root, the ammonium root detects the test paper variable color becomes yellowish-brown, color depth and ammonium radical content are proportionate, and according to shade, contrast the semiquantitative determination that just can carry out the ammonium root with colorimetric card; Described colorimetric card is that the ammonium root detects one group of photochrome or the picture that test paper formed color in the ammonium root solution of normal concentration presents graded.
4, the detection method of ammonium root in breast according to claim 3 and the solution, it is characterized in that: said developer is the OH that contains 1-5mol/L
-NaOH or the deionized water solution of KOH.
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102319800A CN101398387A (en) | 2008-10-28 | 2008-10-28 | Preparation of am detection test paper for milk and solution and am detection method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101806746A (en) * | 2010-04-20 | 2010-08-18 | 内蒙古蒙牛乳业（集团）股份有限公司 | Rapid testing method of zinc salt in milk |
| CN102033063A (en) * | 2010-10-28 | 2011-04-27 | 上海绿帝环保科技有限公司 | Preparation and use method of color comparison detection piece for ammonia nitrogen in water |
| CN102928423A (en) * | 2012-10-25 | 2013-02-13 | 东北制药（沈阳）科技发展有限公司 | Method for detecting ammonium salt in amino-containing medicament |
| CN103149205A (en) * | 2013-02-07 | 2013-06-12 | 顺德出入境检验检疫局 | On-site rapid detection kit for protein adulteration |
| CN105911055A (en) * | 2016-04-29 | 2016-08-31 | 南京信息工程大学 | Method for quickly detecting available nitrogen in soil |
-
2008
- 2008-10-28 CN CNA2008102319800A patent/CN101398387A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101806746A (en) * | 2010-04-20 | 2010-08-18 | 内蒙古蒙牛乳业（集团）股份有限公司 | Rapid testing method of zinc salt in milk |
| CN102033063A (en) * | 2010-10-28 | 2011-04-27 | 上海绿帝环保科技有限公司 | Preparation and use method of color comparison detection piece for ammonia nitrogen in water |
| CN102928423A (en) * | 2012-10-25 | 2013-02-13 | 东北制药（沈阳）科技发展有限公司 | Method for detecting ammonium salt in amino-containing medicament |
| CN102928423B (en) * | 2012-10-25 | 2015-01-21 | 东北制药集团股份有限公司 | Method for detecting ammonium salt in amino-containing medicament |
| CN103149205A (en) * | 2013-02-07 | 2013-06-12 | 顺德出入境检验检疫局 | On-site rapid detection kit for protein adulteration |
| CN105911055A (en) * | 2016-04-29 | 2016-08-31 | 南京信息工程大学 | Method for quickly detecting available nitrogen in soil |
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Open date: 20090401 |