CN107036989B - A method of measurement chrome tanning agent active constituent content - Google Patents
A method of measurement chrome tanning agent active constituent content Download PDFInfo
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- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000470 constituent Substances 0.000 title claims abstract description 41
- 238000005259 measurement Methods 0.000 title claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 136
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 94
- 239000012452 mother liquor Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000002835 absorbance Methods 0.000 claims abstract description 44
- 239000000523 sample Substances 0.000 claims abstract description 44
- 238000012360 testing method Methods 0.000 claims abstract description 42
- 238000002474 experimental method Methods 0.000 claims abstract description 40
- 239000012086 standard solution Substances 0.000 claims abstract description 39
- 239000012153 distilled water Substances 0.000 claims abstract description 37
- 239000012496 blank sample Substances 0.000 claims abstract description 34
- 238000010521 absorption reaction Methods 0.000 claims abstract description 31
- 239000000706 filtrate Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 230000010355 oscillation Effects 0.000 claims description 67
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 44
- 229910052740 iodine Inorganic materials 0.000 claims description 44
- 239000011630 iodine Substances 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 39
- 241001411320 Eriogonum inflatum Species 0.000 claims description 21
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 20
- 238000005303 weighing Methods 0.000 claims description 19
- 238000004090 dissolution Methods 0.000 claims description 12
- 239000004677 Nylon Substances 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 11
- 229920001778 nylon Polymers 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract 1
- 238000011088 calibration curve Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000013068 control sample Substances 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 30
- 229910052804 chromium Inorganic materials 0.000 description 23
- 239000010985 leather Substances 0.000 description 16
- 238000002798 spectrophotometry method Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 102000008186 Collagen Human genes 0.000 description 4
- 108010035532 Collagen Proteins 0.000 description 4
- 229920001436 collagen Polymers 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000209149 Zea Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 229910052711 selenium Inorganic materials 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000003113 alkalizing effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
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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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of methods for measuring chrome tanning agent active constituent content, it is characterized in that method includes the following steps: compound concentration is the chrome tanning agent mother liquor of 2-10 g/L；Utilize the standard solution of mother liquor various concentration；Determine the characteristic absorption wavelength of mother liquor, and at that wavelength using the concentration of standard solution as abscissa, absorbance value is that ordinate draws standard curve, calibration curve coefficient correlation R2Greater than 0.99；Tanning is carried out to chrominated hide powder with mother liquor and is experiment sample with hydrochloric acid or sodium hydroxide adjustment owse pH to 4.0；Skin powder is handled as control sample under the same conditions with acid used in distilled water and adjusting pH or aqueous slkali；Experiment sample and blank sample filtrate is collected by filtration, and at the wavelength of measurement standard curve measurement experiment sample and blank sample filtrate absorbance；The active constituent content of chrome tanning agent is calculated by formula, the difference of parallel test result is less than 1.00%.This method is easy to operate, and repeatability and stability are good, and strong operability can objectively characterize the performance of special chrome tanning agent.
Description
Technical field
The invention belongs to leather chemicals nature examination technical fields, and in particular to a kind of to utilize Spectrophotometric Determination of Chromium
The method of tanning agent active constituent content.
Background technique
Chrome tanning is most popular tannage in current leather industry, the chrome tanning agent Cr used in the process2O3Content one
As be 25 ± 1%.However this kind of chrome tanning agent absorptivity is lower, generally only 60-75%, and there are problems that neutral salt pollution, because
This is proposed the new products such as many high-absorption chrome tanning agent and acid-free chromte tannage agent on the market and is subtracted with improving the absorptivity of chrome tanning agent
Few Chrome Tanning Process pollution (Du Xiaosheng, Lu Lixu, Dan Zhihua, wait the application study of high-selenium corn chromium powder [J] Chinese leather, 2012,
41(7): 6-8；The development of Chen Zhanguang, Chen Wuyong acid-free chromte tannage agent and performance characterization [J] Chinese leather, 2001,30(23):
6-10).In addition, in order to keep chrome tanning agent alkali stability more preferable, the wet blue leather grain of tanning is flat thin, by the way that masking agent production is added
Cover the type chrome tanning agent (MOLECULE DESIGN and development [J] leather science and work of Li Guoying, Zhang Mingrang .KMC series chrome tanning powder of limiting
Journey, 1992,2 (1): 13-21).Meanwhile in order to simplify operation, from alkalizing, chrome tanning agent is also gradually developed and is launched
(novel synthesis [J] from alkalization leather chrome tanning agent of Han Yulin, Xiong Jian finely and specialty chemicals, 1997,17:3-4).Although
The specific nature of chrome tanning agent difference, but the active constituent content of chrome tanning agent is with Cr at present2O3Meter, according to process hides powder
The regulation of shape chrome tanning agent national standard (GB/T24331-2009), Cr in different types of chrome tanning agent2O3Content is both needed to meet certain
Content, such as standard type covers type of limiting, covers and limit cross-linking type and cover the Cr that limits from alkalization type chrome tanning agent2O3Content should be respectively greater than 24%,
23%, 22% and 19%.
Compared with conventional chrome tanning agent, type chrome tanning agent of limiting, certainly alkalization chrome tanning agent, high-absorption chrome tanning agent and acid-free chromte tannage agent are covered
It is intended to add other auxiliary agents in process of production etc. special chrome tanning agent, the addition of auxiliary agent can not only reduce the Cr in chrome tanning agent2O3Contain
Amount, also will increase product cost.With Cr in chrome tanning agent2O3From the point of view of content, type chrome tanning agent of limiting, certainly alkalization chrome tanning agent, high-selenium corn chromium are covered
The Cr such as tanning agent and acid-free chromte tannage agent2O3Content is below conventional chrome tanning agent, but the price of product is then much higher than conventional chrome tanning
Agent, therefore use Cr2O3Content measures the active principle of chrome tanning agent, cannot objectively react the property of special chrome tanning agent, unfavorable
In the popularization of this kind of product.However at present both at home and abroad in addition to using Cr2O3Outside the active constituent content of Content evaluation chrome tanning agent,
The method that he measures chrome tanning agent active constituent content has not been reported.
Summary of the invention
It is single for current measurement chrome tanning agent active constituent content method, and it is unable to the special chrome tanning agent performance of objective expression
Status, inventor is in published chrome tanning agent composition, structure and performance test method and technology and other tanning agents composition, knot
On the basis of structure and performance test methods and technology, the material in conjunction with disclosed in existing chrome tanning technology and chrome tanned mechanics is deeply ground
Study carefully reaction process of the chrome tanning agent in tannery and its action rule with collagen, proposes a kind of measurement chrome tanning
The method of agent active constituent content.
In Chrome Tanning Process, chromium generates tanning effect and forming coordinate bond with the carboxyl dissociated on collagen.
In the process, chromium enters inside leather from owse, shows as chromium content in owse and reduces, chromium content increases in leather.Due to
Leather introduces chromium in tannery, and the quality of leather can be made to increase, and therefore, can theoretically use gravimetric detemination chromium
The effective component of tanning agent.However inventor, by experiment, discovery is of poor quality to characterize chromium before and after tanning by measurement leather
Degree of absorption, so that the method for measuring chrome tanning agent active constituent content is infeasible, main cause are as follows: firstly, since taking
The limitation of sample and laboratory test condition, chrome tanning scale is smaller in detection process, therefore the tanning that can be used for carrying out constant weight is forward and backward
Skin or leather it is also less, this allow for test relative error it is very big；Secondly as the skin or leather moisture content before and after tanning exist
70% or so, therefore constant weight time length, low efficiency, it is not able to satisfy the requirement of enterprise's routine inspection and exfactory inspection；Again, in chromium
During tan, pelt not only absorbs chromium, also absorbs other substances such as neutral salt in chrome tanning agent, and these substances are that do not have
Tanning effect, but its variation that still will lead to leather quality before and after tanning；Finally, due in tannery, it is intradermal
Soluble protein can dissolve out so that after tanning leather weight increase be less than its actual absorption chrome tanning agent in it is effective at
Point, in addition, skin soluble protein content and the amount of dissolution in tannery that different batches experiment uses are inconsistent, so that surveying
Examination repeatability and stability are poor.
Chrome tanning agent solution is blue-green, and there are two characteristic absorption peaks in visible spectral range, is located at the left side 420nm
Right and 580nm or so (Beijing Chen Wuyong, Li Guoying tanning chemistry (third edition) [M]: China Light Industry Press, 2011).
The absorbance of solution and its concentration have linear positive correlation in a certain range, therefore pass through the suction of owse before and after measurement tanning
Luminosity can reflect out the absorbing state of chromium in tannery, characterize the variation of active constituent content in chrome tanning agent.In chrome tanning agent
Neutral salt, masking agent etc. be organic acid and its salt, these substances are not absorbed in visible region, will not cause to do to result
It disturbs；Intracutaneous soluble protein will not still interfere the absorbance of chromium also without visible absorption spectra.Therefore, in certain condition
Under, the absorbance of chrome tanning agent solution is only determined by the content of chromium.Ultraviolet-visible spectrophotometry be carry out constant and
The important method of micro substance assay, this method is easy to operate, and required measured object is few, and error is small, repeatable and stable
Property it is strong, therefore can using ultraviolet-visible spectrophotometry measurement chrome tanning agent active constituent content.
Since different chrome tanning agents composition is different with property, the position of ultraviolet-visible features absorption peak is not also identical,
Before being tested, chrome tanning agent solution is scanned using ultraviolet-visible spectrophotometer first, determines characteristic absorption peak position
It sets, and using this feature absorbing wavelength as the condition of follow-up test, different neutral salt in chrome tanning agent can be eliminated, chromium feature is inhaled
The influence for receiving wavelength is further reduced error, improves measuring accuracy and confidence level.By test of many times, inventor has found chrome tanning
When agent mother liquid concentration is 2-10g/L, make linearly preferable when standard curve, while test result is reproducible and error is smaller.
Meanwhile inventor has found by test of many times, with the chrome tanning agent mother liquor of 0,10,20,30 and 40mL in 100mL volumetric flask, is used in combination
Distilled water is settled to the standard solution that scale system obtains various concentration, and standard solution is measured at pre-determined characteristic absorption wavelength
Absorbance be ordinate, concentration of standard solution be abscissa draw standard curve, standard curve can be with coverage test range, together
When standard curve coefficient R2It is higher, standard curve good linearity.
It is well known that each position fiber weaving conditions of Animal Skin are different, it is poor to there is very big position.Simultaneously as preparing
Workshop section's treatment process, material and raw material skin source are different, and pelt is in tannery to the absorbing state of chromium also difference.
Therefore, inventor replaces pelt to carry out tanning using the standardized pure chrominated hide powder of analysis, can both eliminate pelt position difference to survey
Raw interference is test-manufactured, influence of the pelt source difference to test result is in turn avoided, improve the operability of test and can be weighed
Renaturation.In Chrome Tanning Process, pH value is the key factor for influencing to combine, and different chrome tanning agents is due to molecular composition and structure
Difference, the pH at the end of tanning is also variant, therefore in a kind of measurement chrome tanning agent active constituent content provided by the invention
It in method, needs to adjust tanning system pH to 4.0, so that chromium is adequately in conjunction with collagen, while not making chromium again
It precipitates and is adsorbed on skin, this is the key that Accurate Determining chrome tanning agent active constituent content.
On the basis of the studies above, a kind of method for measuring chrome tanning agent active constituent content is inventor provided, it is special
Sign is to operate the active constituent content that can measure chrome tanning agent by following 7 step:
(1), a certain amount of chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, prepares chromium
Tanning agent concentration is the mother liquor of C g/L, and mother liquid concentration is 2-10g/L；
(2), 0,10,20,30 and 40mL mother liquor is measured respectively and be settled to scale in 100mL volumetric flask, and with distilled water, make
Obtain the standard solution of various concentration；
(3), mother liquor is scanned using ultraviolet-visible spectrophotometer, the characteristic absorption wavelength of mother liquor is determined, at this
The absorbance value of various concentration standard solution is measured under wavelength respectively, and using the concentration of standard solution as abscissa, absorbance value
Standard curve is drawn for ordinate, calculates the slope (K) and related coefficient (R of standard curve2), R20.99 should be greater than；
(4), experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle after mother liquor 100mL is added
Plug comes into full contact with Pi Fenyu mother liquor with hand oscillation, is then put into iodine flask and vibrates 5min into 40 DEG C of water bath chader,
Owse pH to 4.0 is adjusted using the hydrochloric acid or 1mol/L sodium hydroxide solution that concentration is 1mol/L, and records hydrochloric acid or hydroxide
Sodium solution dosage continues thereafter with oscillation 60min；
(5), blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly after distilled water 100mL is added
Bottle stopper comes into full contact with Pi Fenyu distilled water with hand oscillation, then iodine flask is put into 40 DEG C of water bath chader and is vibrated
Hydrochloric acid or sodium hydroxide solution with experiment sample same volume is added in 5min, continues thereafter with oscillation 60min；
(6), it is first filtered using nylon filtering cloth after testing sample and blank sample oscillation, collects filtrate, then filtered with filter paper
Filtrate, filtered filtrate use ultraviolet-visible spectrophotometer measurement experiment sample and sky at the wavelength of measurement standard curve
The absorbance value A of white sample filtrateIt is realAnd AIt is empty；
(7) according to active constituent content (%)=[K × C- (AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective of chrome tanning agent
Component content, test need to carry out parallel test, and the difference of parallel test result is less than 1.00%；
In aforesaid operations, test is distilled water with water, and agents useful for same is analytical reagents in addition to chrome tanning agent.
In a kind of method measuring chrome tanning agent active constituent content provided by the invention, mother liquid concentration is 2-10g/L, female
Liquid characteristic absorption wavelength is any one of 420nm or so characteristic absorption wavelength or 580nm or so characteristic absorption wavelength.The present invention
There is provided a kind of measurement chrome tanning agent active constituent content method can be used for measuring conventional chrome tanning agent, cover limit type chrome tanning agent, from
The active constituent content of any one in alkalization chrome tanning agent, high-absorption chrome tanning agent or acid-free chromte tannage agent.
It is provided by the invention it is a kind of measure chrome tanning agent active constituent content method in, chrome tanning agent mother liquid concentration be 2-
10g/L, the good linearity of subsequent production standard curve, while being also beneficial to the hair of tanning reaction in test process at this concentration
It is raw.Mother liquid concentration is lower than 2 g/L or is higher than 10 g/L, and standard curve is linearly bad, and test result relative error is big.In the present invention
The mother liquor of preparation is 1000mL, can be while meeting test liquid demand, for measuring liquor capacity in rinse test process
Glass apparatus, it is possible to reduce experimental error and the repeatability and confidence level for improving test.The present invention uses 0,10,20,30
With the mother liquor standard solution of 40mL, established standard curve covers test scope, while the related coefficient of standard curve
R2Greater than 0.99, shows that standard curve has good linear relationship, be suitable for quantitative analysis.Although chrome tanning agent solution exists
There are two characteristic absorption peaks at the place 420nm or so and 580nm or so, however due to the difference of chrome tanning agent the Nomenclature Composition and Structure of Complexes, this two
The absorbing wavelength and Relative Absorbance of a characteristic absorption peak can difference, use ultraviolet-visible spectrophotometer before testing
Mother liquor is scanned, determines characteristic absorption peak and corresponding absorbing wavelength, selects the higher characteristic absorption wavelength of Relative Absorbance, in this way
Measurement sensitivity can be improved, reduce error, targetedly the active constituent content of different chrome tanning agents is measured.
In a kind of method for measuring chrome tanning agent active constituent content provided by the invention, skin powder dosage is 10g, when tanning
Mother liquor dosage is 100mL, can obtain relatively large number of filtrate for testing, while filtrate absorbance is also in standard curve range
It is interior.Using 40 DEG C of tannings, and adjusting tanning system pH is 4.0, is the relative parameters setting simulated in conventional Chrome Tanning Process,
It is similar to the actual use situation of chrome tanning agent, the production of test result closing to reality, while tanning effect is good under this condition, chrome tanning agent
In chromium not only can be sufficiently in conjunction with collagen, but also precipitating will not be generated.The adjusting experiment of same volume is added in blank sample
Hydrochloric acid used in sample pH or sodium hydroxide solution can eliminate other substances other than addition chrome tanning agent to the shadow of filtrate absorbance
It rings, improves test accuracy and repeatability.It is tried by the absorbance of test experiments sample and blank sample filtrate, and in parallel
It tests, the difference of parallel test result shows that this method stability is good, reproducibility is high less than 1.00%.
In addition, it also have the advantage that
First, method provided by the invention is easy to operate, and instrument, equipment and reagent are conventional skin material production
Producer laboratory or conventional item on the market, strong operability；
Second, method test result favorable reproducibility provided by the invention, resultant error is small, and measuring stability is strong, surveys simultaneously
Examination speed is fast, and required sample is few, can be used as the test method of routine inspection and exfactory inspection.
Specific embodiment
Embodiment is given below so that the present invention will be described in more detail, it is necessary to be pointed out that following embodiment cannot manage
Solution is limiting the scope of the invention, and the person skilled in the art in the field makes the present invention according to aforementioned present invention content
Some nonessential modifications and adaptations still fall within protection scope of the present invention.
Embodiment 1
A certain amount of conventional chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, prepares chromium
Tanning agent concentration is the mother liquor of 6 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and fixed with distilled water
Hold to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer, in 423nm
At characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and using the concentration of standard solution as abscissa,
Absorbance value is that ordinate draws standard curve, calculates slope of standard curve K and coefficient R2, R2Value is 0.9982；Test sample
Prepare: weighing 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after mother liquor 100mL is added, makes Pi Fenyu with hand oscillation
Mother liquor comes into full contact with, and the use of concentration is 1mol/L after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min
Sodium hydroxide solution to adjust owse pH be 4.0, and record sodium hydroxide solution dosage, continue thereafter with oscillation 60min；Blank sample
Prepare: weighing 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after distilled water 100mL is added, makes skin powder with hand oscillation
It comes into full contact with distilled water, after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is added and experiment sample
The sodium hydroxide solution of same volume continues thereafter with oscillation 60min；It is first filtered, is recycled using nylon filtering cloth after oscillation
Experiment sample and blank sample filtrate are collected in filter paper filtering, and at the wavelength of measurement standard curve, use UV-vis spectroscopy light
The absorbance value A of degree meter measurement experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C- (AIt is real-
AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 2
It weighs a certain amount of illiteracy to limit chrome tanning agent, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, prepares chromium
Tanning agent concentration is the mother liquor of 10 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and fixed with distilled water
Hold to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer, in 585nm
At characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and using the concentration of standard solution as abscissa,
Absorbance value is that ordinate draws standard curve, calculates slope of standard curve K and coefficient R2, R2Value is 0.9968；Test sample
Prepare: weighing in 10.00g chrominated hide powder 250ml iodine flask, cover tightly bottle stopper after mother liquor 100mL is added, makes skin powder and mother with hand oscillation
Liquid comes into full contact with, and the use of concentration is 1mol/L's after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min
It is 4.0 that sodium hydroxide solution, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；Blank calibration
It is standby: to weigh 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after distilled water 100mL is added, make Pi Fenyu with hand oscillation
Distilled water comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is added and experiment sample phase
The sodium hydroxide solution of same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation, recycles filter
Experiment sample and blank sample filtrate are collected in paper filtering, and at the wavelength of measurement standard curve, use spectrophotometry
Count the absorbance value A of measurement experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C- (AIt is real-AIt is empty)]/
(K × C) × 100% calculates the effective component of chrome tanning agent.
Embodiment 3
A certain amount of acid-free chromte tannage agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 8 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 588nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9956；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the sodium hydroxide solution of 1mol/L, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；
Blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added, vibrated with hand
Come into full contact with Pi Fenyu distilled water, then by iodine flask be put into 40 DEG C of water bath chader oscillation 5min after, be added with
The sodium hydroxide solution for testing sample same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation,
Filter paper filtering is recycled, experiment sample and blank sample filtrate are collected, and at the wavelength of measurement standard curve, uses ultraviolet-visible
The absorbance value A of spectrophotometric determination experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C-
(AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 4
A certain amount of alkalization chrome tanning agent certainly is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 2 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 420nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9934；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the hydrochloric acid solution of 1mol/L, which adjusts owse pH, and records hydrochloric acid solution dosage, continues thereafter with oscillation 60min；Blank calibration
It is standby: to weigh 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after distilled water 100mL is added, make Pi Fenyu with hand oscillation
Distilled water comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is added and experiment sample phase
The hydrochloric acid solution of same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation, recycles filter paper mistake
Experiment sample and blank sample filtrate are collected in filter, and at the wavelength of measurement standard curve, are surveyed using ultraviolet-visible spectrophotometer
Surely the absorbance value A of sample and blank sample filtrate is testedIt is realAnd AIt is empty；According to active constituent content (%)=[K × C- (AIt is real-AIt is empty)]/( K×
C) × 100%, the effective component of chrome tanning agent is calculated.
Embodiment 5
A certain amount of high-absorption chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 5 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 584nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9938；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the sodium hydroxide solution of 1mol/L, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；
Blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added, vibrated with hand
Come into full contact with Pi Fenyu distilled water, then by iodine flask be put into 40 DEG C of water bath chader oscillation 5min after, be added with
The sodium hydroxide solution for testing sample same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation,
Filter paper filtering is recycled, experiment sample and blank sample filtrate are collected, and at the wavelength of measurement standard curve, uses ultraviolet-visible
The absorbance value A of spectrophotometric determination experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C-
(AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 6
A certain amount of acid-free chromte tannage agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 4 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 588nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9989；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the sodium hydroxide solution of 1mol/L, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；
Blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added, vibrated with hand
Come into full contact with Pi Fenyu distilled water, then by iodine flask be put into 40 DEG C of water bath chader oscillation 5min after, be added with
The sodium hydroxide solution for testing sample same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation,
Filter paper filtering is recycled, experiment sample and blank sample filtrate are collected, and at the wavelength of measurement standard curve, uses ultraviolet-visible
The absorbance value A of spectrophotometric determination experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C-
(AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 7
A certain amount of high-absorption chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 6 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 580nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9971；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the sodium hydroxide solution of 1mol/L, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；
Blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added, vibrated with hand
Come into full contact with Pi Fenyu distilled water, then by iodine flask be put into 40 DEG C of water bath chader oscillation 5min after, be added with
The sodium hydroxide solution for testing sample same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation,
Filter paper filtering is recycled, experiment sample and blank sample filtrate are collected, and at the wavelength of measurement standard curve, uses ultraviolet-visible
The absorbance value A of spectrophotometric determination experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C-
(AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 8
A certain amount of acid-free chromte tannage agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, is prepared
Chrome tanning agent concentration is the mother liquor of 6 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and uses distilled water
It is settled to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer,
At 587nm characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and is cross with the concentration of standard solution
Coordinate, absorbance value are that ordinate draws standard curve, calculate slope of standard curve K and coefficient R2, R2Value is 0.9982；
Experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, is made with hand oscillation
Pi Fenyu mother liquor comes into full contact with, and after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is using concentration
It is 4.0 that the sodium hydroxide solution of 1mol/L, which adjusts owse pH, and records sodium hydroxide solution dosage, continues thereafter with oscillation 60min；
Blank sample prepares: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added, vibrated with hand
Come into full contact with Pi Fenyu distilled water, then by iodine flask be put into 40 DEG C of water bath chader oscillation 5min after, be added with
The sodium hydroxide solution for testing sample same volume continues thereafter with oscillation 60min；It is first filtered using nylon filtering cloth after oscillation,
Filter paper filtering is recycled, experiment sample and blank sample filtrate are collected, and at the wavelength of measurement standard curve, uses ultraviolet-visible
The absorbance value A of spectrophotometric determination experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C-
(AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
Embodiment 9
A certain amount of conventional chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, prepares chromium
Tanning agent concentration is the mother liquor of 7 g/L；0,10,20,30 and 40mL mother liquor is measured respectively in 100mL volumetric flask, and fixed with distilled water
Hold to scale, the standard solution of various concentration is made；Mother liquor is scanned using ultraviolet-visible spectrophotometer, in 425nm
At characteristic absorption wavelength, the absorbance value of various concentration standard solution is measured respectively, and using the concentration of standard solution as abscissa,
Absorbance value is that ordinate draws standard curve, calculates slope of standard curve K and coefficient R2, R2Value is 0.9921；Test sample
Prepare: weighing 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after mother liquor 100mL is added, makes Pi Fenyu with hand oscillation
Mother liquor comes into full contact with, and the use of concentration is 1mol/L after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min
Sodium hydroxide solution to adjust owse pH be 4.0, and record sodium hydroxide solution dosage, continue thereafter with oscillation 60min；Blank sample
Prepare: weighing 10.00g chrominated hide powder in 250ml iodine flask, cover tightly bottle stopper after distilled water 100mL is added, makes skin powder with hand oscillation
It comes into full contact with distilled water, after iodine flask is then put into 40 DEG C of water bath chader oscillation 5min, is added and experiment sample
The sodium hydroxide solution of same volume continues thereafter with oscillation 60min；It is first filtered, is recycled using nylon filtering cloth after oscillation
Experiment sample and blank sample filtrate are collected in filter paper filtering, and at the wavelength of measurement standard curve, use UV-vis spectroscopy light
The absorbance value A of degree meter measurement experiment sample and blank sample filtrateIt is realAnd AIt is empty；According to active constituent content (%)=[K × C- (AIt is real-
AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent.
For the reproducibility and stability of the method provided by the present invention, the difference of parallel test result is also found in embodiment
Table 1.
Table 1
Claims (6)
1. a kind of method for measuring chrome tanning agent active constituent content, it is characterised in that chrome tanning can be measured by the operation of following 7 step
The active constituent content of agent:
(1), a certain amount of chrome tanning agent is weighed, 1000mL volumetric flask is transferred to after dissolution and is settled to graduation mark, prepares chrome tanning agent
Concentration is the mother liquor of C g/L, and mother liquid concentration is 2-10g/L；
(2), 0,10,20,30 and 40mL mother liquor is measured respectively and be settled to scale in 100mL volumetric flask, and with distilled water, be made not
With the standard solution of concentration；
(3), mother liquor is scanned using ultraviolet-visible spectrophotometer, determines the characteristic absorption wavelength of mother liquor, in the wavelength
The lower absorbance value for measuring various concentration standard solution respectively, and using the concentration of standard solution as abscissa, absorbance value is vertical
Coordinate draws standard curve, calculates the slope K and coefficient R of standard curve2, R20.99 should be greater than；
(4), experiment calibration is standby: weighing 10.00g chrominated hide powder in 250ml iodine flask, covers tightly bottle stopper after mother liquor 100mL is added, uses
Hand oscillation comes into full contact with Pi Fenyu mother liquor, is then put into iodine flask and vibrates 5min into 40 DEG C of water bath chader, uses
The hydrochloric acid or 1mol/L sodium hydroxide solution that concentration is 1mol/L adjust owse pH to 4.0, and record hydrochloric acid or sodium hydroxide is molten
Liquid dosage continues thereafter with oscillation 60min；
(5), blank sample prepares: 10.00g chrominated hide powder is weighed in 250ml iodine flask, covers tightly bottle stopper after distilled water 100mL is added,
Pi Fenyu distilled water is come into full contact with hand oscillation, then iodine flask is put into and vibrates 5min into 40 DEG C of water bath chader,
The hydrochloric acid or sodium hydroxide solution with experiment sample same volume is added, continues thereafter with oscillation 60min；
(6), it tests after sample and blank sample vibrate and is first filtered using nylon filtering cloth, collect filtrate, then with filter paper filter liquor,
Filtered filtrate uses ultraviolet-visible spectrophotometer measurement experiment sample and blank sample at the wavelength of measurement standard curve
The absorbance value A of filtrateIt is realAnd AIt is empty；
(7) according to active constituent content (%)=[K × C- (AIt is real-AIt is empty)]/(K × C) × 100%, calculate the effective component of chrome tanning agent
Content, test need to carry out parallel test, and the difference of parallel test result is less than 1.00%；
In aforesaid operations, test is distilled water with water, and agents useful for same is analytical reagents in addition to chrome tanning agent.
2. a kind of method for measuring chrome tanning agent active constituent content according to claim 1, it is characterised in that chrome tanning agent is
Conventional chrome tanning agent.
3. a kind of method for measuring chrome tanning agent active constituent content according to claim 1, it is characterised in that chrome tanning agent is
Illiteracy is limited type chrome tanning agent.
4. a kind of method for measuring chrome tanning agent active constituent content according to claim 1, it is characterised in that chrome tanning agent is
From alkalization chrome tanning agent.
5. a kind of method for measuring chrome tanning agent active constituent content according to claim 1, it is characterised in that chrome tanning agent is
High-absorption chrome tanning agent.
6. a kind of method for measuring chrome tanning agent active constituent content according to claim 1, it is characterised in that chrome tanning agent is
Acid-free chromte tannage agent.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0564948A1 (en) * | 1992-04-09 | 1993-10-13 | Nalco Chemical Company | Ultraviolet spectrographic monitoring of water soluble corrosion inhibitors |
| CN1959376A (en) * | 2005-11-03 | 2007-05-09 | 牛增元 | Method for detecting hexavalent chrome in dyed leather and product |
| CN106092921A (en) * | 2016-05-31 | 2016-11-09 | 无锡伊佩克科技有限公司 | The detection method of hexavalent chromium content in a kind of passivating solution |
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|---|---|---|---|---|
| EP0564948A1 (en) * | 1992-04-09 | 1993-10-13 | Nalco Chemical Company | Ultraviolet spectrographic monitoring of water soluble corrosion inhibitors |
| CN1959376A (en) * | 2005-11-03 | 2007-05-09 | 牛增元 | Method for detecting hexavalent chrome in dyed leather and product |
| CN106092921A (en) * | 2016-05-31 | 2016-11-09 | 无锡伊佩克科技有限公司 | The detection method of hexavalent chromium content in a kind of passivating solution |
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