CN107703076A - The assay method of iron content in a kind of pit mud - Google Patents
The assay method of iron content in a kind of pit mud Download PDFInfo
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- CN107703076A CN107703076A CN201711036400.8A CN201711036400A CN107703076A CN 107703076 A CN107703076 A CN 107703076A CN 201711036400 A CN201711036400 A CN 201711036400A CN 107703076 A CN107703076 A CN 107703076A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention discloses a kind of assay method of iron content in pit mud, it is related to constituent content mensure technical field, comprises the following steps：1) sample pretreatment；2) preparation of iron standard items；3) determination of maximum absorption wavelength；4) foundation of iron standard curve；5) in pit mud sample iron content measure.Using method provided by the present invention, color developing effect is good, and the accurate measure of content of trace iron in pit mud can be achieved.Detection method color stability is good used by detection method measure provided by the invention, can accurately determine iron content in pit mud；In the detection method of use, have analyze speed fast, the degree of accuracy is high, the characteristics of favorable reproducibility；The iron content standard that the present invention determines, strong data supporting is provided to pit mud quality system appraisal, pit maintenance and culture of artificial pit mud.
Description
Technical field
The present invention relates to constituent content mensure technical field, and in particular to the assay method of iron content in a kind of pit mud.
Background technology
With the development of the social economy, white wine closely has thousands of years as the consumer goods common in daily life in China
Development history, as the distinctive Conventional espresso wine of China, traditional brewage process be mainly produce with obvious characteristic it is dense,
Clearly, sauce, meter Si great aromatic white spirits.Contain a large amount of microorganisms in pit mud, these microorganisms participate in the brewing process of white wine.
But pit mud is after a long time use, it may occur that aging phenomenon, surface salinization of soil, hardened and hard, water content is few,
Water permeability is gradually reduced, and by pit mud surface is slow and inner development, white powder or elongate can be progressively produced inside pit mud
Crystallization, influence the effect of wine brewing.Analyzed through relevant scientific research institution, white powder material is calcium lactate, and elongated acicular crystal is
Ferrous lactate, wherein ferrous lactate have strong toxic action to microorganism.The general content using iron in directly measure pit mud,
And then it is inferred to the content of ferrous lactate, but the iron content of this low content determines, common measuring method is relatively simple, and
And caused error is larger, actual pit mud processing is easily influenceed.
The content of the invention
The present invention is precisely in order to avoid the weak point present in above-mentioned prior art, there is provided a kind of
The present invention adopts the following technical scheme that to solve technical problem：The assay method of iron content in a kind of pit mud, including
Following steps：
1) sample pretreatment：Pit mud sample is taken in pit, is air-dried after pulverizing, 40-80 mesh sieves for subsequent use；
2) preparation of iron standard items：It is 100mg/L iron standard solutions to be configured to concentration；
3) determination of maximum absorption wavelength：The iron standard solution prepared in step 2) is taken, is developed the color according to coloration method, is used
Ultraviolet-visible spectrophotometer scans in the range of 400-700nm, determines maximum absorption wavelength 510nm.
4) foundation of iron standard curve：Some groups of the iron standard solution prepared in step 2) is measured respectively, according to aobvious
After color method colour developing, light absorption value is determined at maximum wavelength, using iron standard concentration as abscissa x, light absorption value is ordinate y,
Establish standard curve；
5) in pit mud sample iron content measure：The pit mud sample after step 1) processing is taken, extraction solution is added, filters to take
Clear liquid, add the iron that the abundant dissolved oxygen of sodium hydrate aqueous solution is shaken into clear liquid and precipitate completely, then filtered by filter membrane, make precipitation
Iron is filtered to filter membrane, takes filter membrane to be placed in 25mL colorimetric cylinder, and adds 10-15mL sodium acetate solution, makes precipitation complete
Dissolving, take out filter membrane；Hydroxylamine hydrochloride solution 1-4mL, developer Phen 0.5-3mL are added into colorimetric cylinder again, is mixed, it is fixed
Appearance, colour developing balance 10-20min, it is that light absorption value is determined at 510nm in wavelength, according to standard curve, iron contains in calculating sample
Amount.
Further, extraction solution is the second that substance withdrawl syndrome is 0.5-2mol/L, pH value is 3-5 in the step 5)
Acid sodium aqueous solution.
Further, extracting method is that normal temperature shakes or 20-40min is rocked in 40 DEG C of water-baths in the step 5).
Further, sodium hydrate aqueous solution substance withdrawl syndrome is 0.5-2mol/L in the step 5).
Further, the miillpore filter that the micropore of filter membrane is 0.45 μm or 0.22 μm in the step 5).
Further, hydroxylamine hydrochloride concentration is the 5%-20% aqueous solution in the step 5), and Phen concentration is
The 0.1%-0.5% aqueous solution.
Further, in the step 4), the equation of linear regression of standard curve is：Y=0.196x+0.001, R2=
0.999981, linear concentration scope is 0-5mg/L.
The invention provides a kind of assay method of iron content in pit mud, have the advantages that：
1st, detection method color stability is good used by detection method measure provided by the invention, can accurately determine pit mud
Middle iron content；
2nd, in the detection method that uses of the present invention, have analyze speed fast, the degree of accuracy is high, the characteristics of favorable reproducibility；
3rd, the iron content standard that the present invention determines, to pit mud quality system appraisal, pit maintenance and culture of artificial pit mud
Strong data supporting is provided.
Brief description of the drawings
Fig. 1 is absorbance curve of the iron standard liquid in 400-700nm wave-length coverages.
Fig. 2 is the standard curve of iron.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Embodiment：
The assay method of iron content, specific embodiment are as follows in pit mud：
The assay method of iron content, comprises the following steps in a kind of pit mud：
1) sample pretreatment：Pit mud sample is taken in pit, is air-dried after pulverizing, 40-80 mesh sieves for subsequent use；
2) preparation of iron standard items：50mg iron ammonium sulfates are taken, in 500mL clean beakers, first add 300mL distilled waters
After stirring and dissolving, it is 3 to adjust pH value with hydrochloric acid, and then with 500mL volumetric flask constant volumes, it is 100mg/L iron standard items to be configured to concentration
Solution；
3) determination of maximum absorption wavelength：The iron standard solution prepared in step 2) is taken, is developed the color according to coloration method, is used
Ultraviolet-visible spectrophotometer scans in the range of 400-700nm, determines a length of 510nm of maximum absorption wave, that is, obtains iron mark
Absorbance curve of the quasi- solution in 400-700nm wave-length coverages is as shown in Figure 1.
4) foundation of iron standard curve：Measure respectively the iron standard solution 0 prepared in step 2), 0.5mL, 1.0mL,
1.5mL, 2.0mL, 2.5mL are in 50mL volumetric flasks, and after being developed the color according to coloration method, light absorption value is determined at maximum wavelength, with
Iron standard concentration is abscissa x, and light absorption value is ordinate y, establishes standard curve, as shown in Figure 2；
5) in pit mud sample iron content measure：The pit mud of 4 mouthfuls of pits is taken, precision weighs 4.000g samples in 3 respectively
In 50mL colorimetric cylinders, addition 40mL substance withdrawl syndromes are 0.5-2mol/L, the sodium acetate solution that pH value is 3-5, normal temperature concussion
Or 20-40min is rocked in 40 DEG C of water-baths, after being filtered with qualitative filter paper, clear liquid 25mL is taken respectively, adds appropriate substance withdrawl syndrome
20-40min is shaken for the abundant dissolved oxygen of 0.5-2mol/L sodium hydrate aqueous solutions, precipitates the iron in extract solution complete, is passing through
0.45 μm or 0.22 μm of filter membrane suction filtration, make precipitated iron filter to filter membrane, take filter membrane, be added in 25mL colorimetric cylinder, add
The sodium acetate solution that 10-15mL substance withdrawl syndrome is 0.5-2mol/L, pH value is 3-5, is completely dissolved precipitation, takes out filter
Film；It is that 5%-20% hydroxylamine hydrochloride solutions 1-4mL makes ferric iron back be divalence to add concentration thereto, then is added thereto
0.5-3mL concentration is 0.1%-0.5% Phen developer, is mixed, constant volume, colour developing balance 10-20min, is in wavelength
Light absorption value is determined at 510nm, according to standard curve, calculates the content of iron in sample.
According to above-mentioned experimental procedure, iron content such as table 1 below in measured part aged pit mud：
Table 1
| Pit is numbered | Light absorption value | Concentration mg/L | Equivalent (mg/kg pit muds) |
| 1 | 0.2742 | 1.394 | 13.94 |
| 2 | 0.1737 | 0.8814 | 8.814 |
| 3 | 0.2815 | 1.431 | 14.31 |
| 4 | 0.2503 | 1.2719 | 12.719 |
Mensuration methodology is investigated
1) precision test
The pit mud sample not the air-dried portion of a certain pit kind is taken, extract, filter according to the method for invention offer, precipitating,
After dissolving, then developed the color, determine its absorbance, be repeated 6 times, measure RSD absorbances as 0.044 such as table 2 below.
The Precision test result of table 2：
Table 2
2) reappearance is tested
46th, take and pass through 6 parts air-dried of pit mud sample equivalent in same pit, extract, filter according to the method described above, precipitating,
After dissolving, developed the color by the above process, determine its absorbance respectively, try to achieve absorbance RSD values as 4.300 such as table 3 below.
47th, the pit mud iron reappearance experimental result of table 3：
Table 3
3) stability experiment
Take and pit mud sample is air-dried in same pit, extract, filter according to the method described above, precipitating, after dissolving, by the above process
Developed the color, absorbance is determined after placing 0,1h, 2h, 3h, 4h and 5h, try to achieve absorbance RSD values as 0.094 such as table 4 below.
Table 4 surveys pit mud iron stability experimental result：
Table 4
Recovery of standard addition is tested：
Take 3 pit mud samples, extract, filter according to the method described above, precipitation, after dissolving, each sample grades 3 parts of volume,
The iron standard items (10mg/L) of 1mL, 2mL and 3mL concentration known are separately added into, after mixing, are developed the color by the above process, are surveyed
Determine absorbance, calculating average recovery rate is 98.58%, RSD 3.08.
The recovery of standard addition experimental result of the pit mud iron of table 5：
Table 5
In summary, 1, detection method color stability is good used by detection method provided by the invention measure, can essence
Really iron content in measure pit mud.
2nd, in the detection method that the present invention uses, existing will be fast with analyze speed, and the degree of accuracy is high, the spy of favorable reproducibility
Point.
3rd, the iron content standard that the present invention determines, to pit mud quality system appraisal, pit maintenance and culture of artificial pit mud
Strong data supporting is provided.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply and deposited between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements not only will including those
Element, but also the other element including being not expressly set out, or it is this process, method, article or equipment also to include
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Other identical element also be present in process, method, article or equipment including the key element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (7)
- A kind of 1. assay method of iron content in pit mud, it is characterised in that：Comprise the following steps：1) sample pretreatment：Pit mud sample is taken in pit, is air-dried after pulverizing, 40-80 mesh sieves for subsequent use；2) preparation of iron standard items：It is 100mg/L iron standard solutions to be configured to concentration；3) determination of maximum absorption wavelength：The iron standard solution prepared in step 2) is taken, is developed the color according to coloration method, with purple Outside-visible spectrophotometer scans in the range of 400-700nm, determines maximum absorption wavelength 510nm.4) foundation of iron standard curve：Some groups of the iron standard solution prepared in step 2) is measured respectively, according to colour developing side After method colour developing, light absorption value is determined at maximum wavelength, using iron standard concentration as abscissa x, light absorption value is ordinate y, is established Standard curve；5) in pit mud sample iron content measure：The pit mud sample after step 1) processing is taken, adds extraction solution, is filtered to take clear Liquid, add the iron that the abundant dissolved oxygen of sodium hydrate aqueous solution is shaken into clear liquid and precipitate completely, then filtered by filter membrane, make precipitated iron On filtering to filter membrane, take filter membrane to be placed in 25mL colorimetric cylinder, and add 10-15mL sodium acetate solution, make precipitation completely molten Solution, take out filter membrane；Hydroxylamine hydrochloride solution 1-4mL, developer Phen 0.5-3mL are added into colorimetric cylinder again, is mixed, it is fixed Appearance, colour developing balance 10-20min, it is that light absorption value is determined at 510nm in wavelength, according to standard curve, iron contains in calculating sample Amount.
- 2. the assay method of iron content in the pit mud according to claims 1, it is characterised in that extracted in the step 5) Solution is the aqueous sodium acetate solution that substance withdrawl syndrome is 0.5-2mol/L, pH value is 3-5.
- 3. the assay method of iron content in the pit mud according to claims 1, it is characterised in that extracted in the step 5) Method is that normal temperature shakes or 20-40min is rocked in 40 DEG C of water-baths.
- 4. according to the method described in claims 1, it is characterised in that the amount of sodium hydrate aqueous solution material in the step 5) Concentration is 0.5-2mol/L.
- 5. according to the method described in claims 1, it is characterised in that in the step 5) micropore of filter membrane be 0.45 μm or 0.22 μm of miillpore filter.
- 6. according to the method described in claims 1, it is characterised in that hydroxylamine hydrochloride concentration is 5%-20% in the step 5) The aqueous solution, Phen concentration be 0.1%-0.5% the aqueous solution.
- 7. according to the method described in claims 1, it is characterised in that in the step 4), the linear regression side of standard curve Cheng Wei：Y=0.196x+0.001, R2=0.999981, linear concentration scope are 0-5mg/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111007027A (en) * | 2019-12-31 | 2020-04-14 | 濮阳宏业环保新材料股份有限公司 | Method for measuring iron content in thiourea dioxide |
| CN112853255A (en) * | 2020-12-31 | 2021-05-28 | 西安优耐特容器制造有限公司 | Zirconium-based material surface in-situ ceramic composite treatment method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101738391A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院沈阳应用生态研究所 | Mensuration method for amorphous Fe in soil |
| CN101975688A (en) * | 2010-09-29 | 2011-02-16 | 山西潞安矿业(集团)有限责任公司 | Sample pretreatment method for determining iron content in oil |
| CN102323257A (en) * | 2011-06-02 | 2012-01-18 | 广州科城环保科技有限公司 | Method for detecting trace iron in copper sulfate |
| CN102494974A (en) * | 2011-12-07 | 2012-06-13 | 西南科技大学 | Evaluation method-wettability measuring method for pit mud |
-
2017
- 2017-10-30 CN CN201711036400.8A patent/CN107703076A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101738391A (en) * | 2008-11-12 | 2010-06-16 | 中国科学院沈阳应用生态研究所 | Mensuration method for amorphous Fe in soil |
| CN101975688A (en) * | 2010-09-29 | 2011-02-16 | 山西潞安矿业(集团)有限责任公司 | Sample pretreatment method for determining iron content in oil |
| CN102323257A (en) * | 2011-06-02 | 2012-01-18 | 广州科城环保科技有限公司 | Method for detecting trace iron in copper sulfate |
| CN102494974A (en) * | 2011-12-07 | 2012-06-13 | 西南科技大学 | Evaluation method-wettability measuring method for pit mud |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111007027A (en) * | 2019-12-31 | 2020-04-14 | 濮阳宏业环保新材料股份有限公司 | Method for measuring iron content in thiourea dioxide |
| CN112853255A (en) * | 2020-12-31 | 2021-05-28 | 西安优耐特容器制造有限公司 | Zirconium-based material surface in-situ ceramic composite treatment method |
| CN112853255B (en) * | 2020-12-31 | 2024-03-15 | 西安优耐特容器制造有限公司 | Zirconium-based material surface in-situ ceramic composite treatment method |
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Application publication date: 20180216 |