CN113432944B - Method for removing hematoxylin dye for silk strontium isotope detection - Google Patents
Method for removing hematoxylin dye for silk strontium isotope detection Download PDFInfo
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- CN113432944B CN113432944B CN202110686873.2A CN202110686873A CN113432944B CN 113432944 B CN113432944 B CN 113432944B CN 202110686873 A CN202110686873 A CN 202110686873A CN 113432944 B CN113432944 B CN 113432944B
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- deionized water
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- 238000000034 method Methods 0.000 title claims abstract description 26
- WZUVPPKBWHMQCE-UHFFFAOYSA-N Haematoxylin Chemical compound C12=CC(O)=C(O)C=C2CC2(O)C1C1=CC=C(O)C(O)=C1OC2 WZUVPPKBWHMQCE-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000001514 detection method Methods 0.000 title claims abstract description 9
- 229910052712 strontium Inorganic materials 0.000 title claims abstract description 9
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 title claims abstract description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 9
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 235000015162 Caesalpinia sappan Nutrition 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 238000011049 filling Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229940037003 alum Drugs 0.000 claims description 10
- 235000011126 aluminium potassium sulphate Nutrition 0.000 claims description 10
- LCPUDZUWZDSKMX-UHFFFAOYSA-K azane;hydrogen sulfate;iron(3+);sulfate;dodecahydrate Chemical compound [NH4+].O.O.O.O.O.O.O.O.O.O.O.O.[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCPUDZUWZDSKMX-UHFFFAOYSA-K 0.000 claims description 10
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 239000011651 chromium Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 229940050271 potassium alum Drugs 0.000 claims description 10
- GNHOJBNSNUXZQA-UHFFFAOYSA-J potassium aluminium sulfate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GNHOJBNSNUXZQA-UHFFFAOYSA-J 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 6
- 101100328463 Mus musculus Cmya5 gene Proteins 0.000 claims description 5
- LRSYPTQGLVXIBF-UHFFFAOYSA-N [C].[Sr] Chemical compound [C].[Sr] LRSYPTQGLVXIBF-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000000176 thermal ionisation mass spectrometry Methods 0.000 claims description 5
- 238000013055 trapped ion mobility spectrometry Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 241000209639 Biancaea sappan Species 0.000 claims 4
- 238000004043 dyeing Methods 0.000 abstract description 12
- 239000004744 fabric Substances 0.000 abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 244000306301 Caesalpinia sappan Species 0.000 description 24
- 238000011160 research Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009933 burial Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000003438 strontium compounds Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
Abstract
The invention relates to the technical field of cultural relic detection and discloses a method for removing hematoxylin dye for silk strontium isotope detection. The method adopts hydrofluoric acid and sodium hypochlorite solution, and the two reagents are common, have low cost, are safe and nontoxic, can not damage fabrics, are convenient to operate, are easy to treat at the residual night, and can not pollute the environment. The invention has the creativity that aiming at the hematoxylin dye to imitate the ancient silk dyeing process, the influence rule of the hematoxylin on the silk stable isotope value in the dyeing process is found, the influence of the dye is eliminated by finding out the corresponding method, the invention has great practical significance, and an important foundation can be further laid for tracing the source production place of silk relics by isotopes.
Description
Technical Field
The invention relates to the technical field of cultural relic detection, in particular to a method for removing hematoxylin dye for silk strontium isotope detection.
Background
Silk is historically the first global commodity and the source of silk cultural relics has been the direction of research for more than a hundred years by historians and archaeologists. At present, the tracing of the production place of the silk fabrics by using stable isotopes is a more accurate method system for tracing the textile relics, and also belongs to the development direction of scientifically developing the tracing of the isotope technology of the textile relics. However, to trace the origin of silk by using isotope technology, the influence of the whole process from mulberry leaves, cocoons to finished products on isotopes needs to be explored, which is essential for the study of the ancient silk dyeing and finishing process. Silk is a type of exogenous saw in fabrics that has been carried into many environments by dyeing and storage in different places, burial, etc. Exogenous strontium has great interference effect on tracking and tracing research of archaeological textiles, so that saw isotope tracking research can be performed only by removing exogenous strontium.
The hematoxylin is used as a natural plant dye commonly used for ancient silk dyeing, and stable isotope research is carried out on the hematoxylin-dyed silk, so that the isotope change rule in the process is obtained, the method has high practical significance, and an important foundation can be further laid for isotope tracing of the source production place of silk relics.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for removing hematoxylin dye for silk strontium isotope detection. The dyeing liquid extracted from sappan wood by adopting an ancient method dyeing process is used for dyeing silk, hydrofluoric acid is used for dissolving a part of particles attached to fibers, and then sodium hypochlorite solution is mixed for further dissolving strontium compounds. The method adopts hydrofluoric acid and sodium hypochlorite solution, is safe and nontoxic, does not damage fabrics, is convenient to operate, is easy to treat residual liquid, and does not pollute the environment.
The specific technical scheme of the invention is as follows: a method for removing hematoxylin dye for silk strontium isotope detection comprises the following steps:
1) Placing massive natural sappan wood in a container, adding deionized water, soaking at 20-30deg.C for 20-40min, drying, pulverizing sappan wood into powder, and placing into a sample bottle for testing;
2) Weighing deionized water, pouring the deionized water into a sample bottle, and soaking the sample bottle for 6-8 hours at 20-30 ℃;
3) Placing the sample bottle in a constant temperature heating stirrer, heating to 35-45deg.C, adding Na 2 CO 3 Continuously heating to 75-85deg.C, stirring at constant temperature for 50-70min, vacuum filtering, pouring the residue into sample bottle, and collecting filtrate as Sucus Caesalpiniae sappan;
4) Repeating the step 3) twice to obtain two sappan wood juice and three sappan wood juice; finally, drying filter residues, and filling the filter residues into a self-sealing bag to be tested;
5) Uniformly mixing the first sappan juice, the second sappan juice and the third sappan juice to obtain mixed dye liquor, carrying out suction filtration, adjusting the pH of the dye liquor to 6-7 by using acetic acid solution, and placing the dye liquor in a centrifuge tube to be tested;
6) Weighing 20-25 g of blank silk sample, cutting into a plurality of pieces, soaking in a cleaning solution, taking out, cleaning with deionized water, taking a piece of cleaned blank silk sample, naturally air-drying, and filling into a self-sealing bag to be tested;
7) Taking 4 beakers, the number of which is A, B, C, D, measuring the dye liquor in the step 5) by each beaker, and weighing natural iron alum, potassium alum and chromium alum which are taken as mordants to be respectively added into the B, C, D beakers;
8) Placing the 4 beakers in a constant-temperature heating stirrer, heating while stirring, when the temperature is raised to 35-45 ℃, placing a piece of silk into each beakers until the mordant is fully dissolved, continuously heating to 75-85 ℃, stirring for 40-50min, washing with 35-45 ℃ deionized water, naturally air-drying a sappan-dyed silk sample, and placing the sappan-dyed silk sample into a self-sealing bag for testing;
9) Preparing 4 beakers, respectively pouring hydrofluoric acid solution into the beakers, respectively putting 4 sappan-dyed silk samples into the 4 beakers, stirring, slowly pouring sodium hypochlorite solution while stirring, taking out the sappan-dyed silk samples after 55-65 min, washing with deionized water, and airing;
10 And (3) detecting the isotope of the strontium carbon nitride of the oxyhydroxide by using TIMS for the samples to be detected obtained in the steps 1), 3), 4), 5), 7), 8) and 9).
Preferably, in the step 1), the mass of the sappan wood is 30-38 g, and the deionized water is 500-1000mL.
Preferably, in step 2), the deionized water has a volume of 250-350mL.
Preferably, in step 3), the Na 2 CO 3 The mass of (2) is 1.5-2.0 g.
Preferably, in the step 5), the concentration of the acetic acid solution is 8-12wt%, and 40-60mL of dye liquor is taken out from the centrifuge tube to be measured.
Preferably, in the step 6), the mass of the blank silk sample is 20-25 g, the blank silk sample is cut into 4 pieces, the size is 20.0cm multiplied by 20.0cm, the volume ratio of water to ethanol in the used cleaning solution is 1:1, and the blank silk sample is soaked for 20-40min.
Preferably, in the step 7), each beaker is used for measuring 250-300 mL of the dye liquor in the step 5, and 1.25-1.5 g of natural iron alum, potassium alum and chromium alum are respectively weighed.
Preferably, in the step 9), the volumes of the hydrofluoric acid solution poured into the 4 beakers are 250-300 mL, the concentration is 1mol/L, the volume of the sodium hypochlorite solution slowly poured into the beakers while stirring is 40-60mL, the concentration is 5wt%, and the sample cloth is taken out after 55-65 min, washed by deionized water and dried.
Compared with the prior art, the invention has the beneficial effects that:
(1) The stable isotope technology is adopted to carry out traceability research on silk dyed by the sappan archaizing process, the stable isotope value of the silk sample at each step in the dyeing process and the stable isotope in the dye liquor sample are measured, and finally, the result is analyzed to trace the origin of the silk.
(2) The adopted dyeing raw materials are natural raw materials, are not processed, highly imitate the process steps of ancient sappan wood for dyeing silk, and have important practical significance.
(3) And detecting and analyzing the sample intercepted in the dyeing process by adopting a method of combining various isotope information.
(4) Few kinds of chemical reagents are used, the subsequent treatment of the residual night is simpler, and the environment is not polluted. The preparation of the reagent is also very simple.
Drawings
FIG. 1 is a photograph of a Yunnan sappan wood stained silk sample obtained in example 1;
FIG. 2 is a photograph of a Guangxi sappan-stained silk sample obtained in example 2.
Detailed Description
Example 1
1) Weighing 30g of small natural sappan wood blocks, putting into a beaker, adding 500mL of deionized water, soaking for 30min at 25 ℃, placing into an oven for drying, crushing sappan wood into powder by a multifunctional crusher, and putting 4g of sappan wood powder into the beaker to be tested.
2) 300mL of deionized water was weighed into the second beaker described in step 1 and soaked at 25℃for 6 hours.
3) The beaker of step 2 was placed in a thermostatically heated magnetic stirrer and 1.5g of Na was added when the temperature was raised to 40℃ 2 CO 3 Continuously heating to 80 ℃, stirring at constant temperature for 60min, filtering while the mixture is hot, pouring filter residues back into a beaker, and keeping filtrate as Sucus sappan.
4) And repeating the step 3 for two times, wherein the deionized water is added for 300mL each time, and the two-juice and three-juice of sappan wood can be obtained. And finally, drying the filter residues, and filling the filter residues into a self-sealing bag to be tested.
5) Uniformly mixing the first sappan juice, the second sappan juice and the third sappan juice to obtain mixed dye liquor, carrying out suction filtration, and regulating the pH of the dye liquor to 6 by using an acetic acid solution with the concentration of 10%. 50mL of dye liquor is taken out of the centrifuge tube to be measured.
6) Weighing 20g of blank silk sample, cutting into 4 pieces with the size of 20.0cm multiplied by 20.0cm, soaking in a proper amount of cleaning solution (water/ethanol=1/1) for 30min, taking out the silk sample, and cleaning with deionized water. And (5) taking a piece of clean blank silk, naturally airing, and filling into a self-sealing bag to be tested.
7) Taking 4 beakers, with the number of A, B, C, D, taking 250mL of the dye liquor in the step 5 by each beaker, weighing 1.25g of natural iron alum, potassium alum and chromium alum as mordants, and adding the natural iron alum, potassium alum and chromium alum into the B, C, D beakers respectively.
8) Placing the 4 beakers in a constant-temperature heating magnetic stirrer, heating while stirring, and when the temperature is raised to 40 ℃, placing a piece of silk into each beakers until the mordant is fully dissolved, continuously heating to 80 ℃, stirring for 45min, and washing with deionized water at 40 ℃. And (5) naturally air-drying the sappan wood dyed silk sample, and then filling the sample into a self-sealing bag to be tested.
9) Preparing 4 beakers, pouring 250mL of 1mol/L hydrofluoric acid solution respectively, putting 4 pieces of sample cloth into the 4 beakers respectively, stirring for 20min, slowly pouring 40mL of 5wt% sodium hypochlorite solution under stirring, taking out the sample cloth after 55min, washing with deionized water, and airing.
10 And (3) detecting the isotope of the strontium carbon nitride of the sample by adopting TIMS to the sample to be detected in the steps 1, 3, 4, 5, 7, 8 and 9.
FIG. 1A photograph of a Yunnan sappan wood stained silk sample obtained in example 1.
Example 2
1) Weighing 40g of small natural sappan wood blocks, putting into a beaker, adding 750mL of deionized water, soaking for 30min at 25 ℃, placing into an oven for drying, crushing sappan wood into powder by a multifunctional crusher, and putting 4g of sappan wood powder into the beaker to be tested.
2) 500mL of deionized water was weighed into the second beaker described in step 1 and soaked at 25℃for 8 hours.
3) The beaker of step 2 was placed in a constant temperature heated magnetic stirrer and 2.0g of Na was added when the temperature was raised to 40℃ 2 CO 3 Continuously heating to 80 ℃, stirring at constant temperature for 60min, filtering while the mixture is hot, pouring filter residues back into a beaker, and keeping filtrate as Sucus sappan.
4) And repeating the step 3 for two times, wherein the deionized water is added for 300mL each time, and the two-juice and three-juice of sappan wood can be obtained. And finally, drying the filter residues, and filling the filter residues into a self-sealing bag to be tested.
5) Uniformly mixing the first sappan juice, the second sappan juice and the third sappan juice to obtain mixed dye liquor, carrying out suction filtration, and regulating the pH of the dye liquor to 7 by using an acetic acid solution with the concentration of 10%. 50mL of dye liquor is taken out of the centrifuge tube to be measured.
6) Weighing 25g of blank silk sample, cutting into 4 pieces with the size of 20.0cm multiplied by 20.0cm, soaking in a proper amount of cleaning solution (water/ethanol=1/1) for 30min, taking out the silk sample, and cleaning with deionized water. And (5) taking a piece of clean blank silk, naturally airing, and filling into a self-sealing bag to be tested.
7) Taking 4 beakers, with the number of A, B, C, D, taking 300mL of the dye liquor in the step 5 by each beaker, weighing 1.5g of natural iron alum, potassium alum and chromium alum as mordants, and adding the natural iron alum, potassium alum and chromium alum into the B, C, D beakers respectively.
8) Placing the 4 beakers in a constant-temperature heating magnetic stirrer, heating while stirring, and when the temperature is raised to 40 ℃, placing a piece of silk into each beakers until the mordant is fully dissolved, continuously heating to 80 ℃, stirring for 45min, and washing with deionized water at 40 ℃. And (5) naturally air-drying the sappan wood dyed silk sample, and then filling the sample into a self-sealing bag to be tested.
9) Preparing 4 beakers, pouring 300mL of 1mol/L hydrofluoric acid solution respectively, putting 4 pieces of sample cloth into the 4 beakers respectively, stirring for 20min, slowly pouring 60mL of 5wt% sodium hypochlorite solution under stirring, taking out the sample cloth after 65min, washing with deionized water, and airing.
10 And (3) detecting the isotope of the strontium carbon nitride of the sample by adopting TIMS to the sample to be detected in the steps 1, 3, 4, 5, 7, 8 and 9.
FIG. 2A photograph of a Guangxi sappan-stained silk sample obtained in example 2.
Example 3
1) Weighing 50g of small natural sappan wood blocks, putting into a beaker, adding 1000mL of deionized water, soaking for 30min at 25 ℃, placing into an oven for drying, crushing sappan wood into powder by a multifunctional crusher, and loading 4g of sappan wood powder into the beaker to be tested.
2) 400mL of deionized water was weighed into the second beaker described in step 1 and soaked at 25℃for 7 hours.
3) The beaker of step 2 was placed in a thermostatically heated magnetic stirrer and 1.5g of Na was added when the temperature was raised to 40℃ 2 CO 3 Continuously heating to 80 ℃, stirring at constant temperature for 60min, filtering while the mixture is hot, pouring filter residues back into a beaker, and keeping filtrate as Sucus sappan.
4) And repeating the step 3 for two times, wherein the deionized water is added for 300mL each time, and the two-juice and three-juice of sappan wood can be obtained. And finally, drying the filter residues, and filling the filter residues into a self-sealing bag to be tested.
5) Uniformly mixing the first sappan juice, the second sappan juice and the third sappan juice to obtain mixed dye liquor, carrying out suction filtration, and regulating the pH of the dye liquor to 6.5 by using an acetic acid solution with the concentration of 10%. 50mL of dye liquor is taken out of the centrifuge tube to be measured.
6) Weighing 20g of blank silk sample, cutting into 4 pieces with the size of 20.0cm multiplied by 20.0cm, soaking in a proper amount of cleaning solution (water/ethanol=1/1) for 30min, taking out the silk sample, and cleaning with deionized water. And (5) taking a piece of clean blank silk, naturally airing, and filling into a self-sealing bag to be tested.
7) Taking 4 beakers, with the number of A, B, C, D, taking 250mL of the dye liquor in the step 5 by each beaker, weighing 1.25g of natural iron alum, potassium alum and chromium alum as mordants, and adding the natural iron alum, potassium alum and chromium alum into the B, C, D beakers respectively.
8) Placing the 4 beakers in a constant-temperature heating magnetic stirrer, heating while stirring, and when the temperature is raised to 40 ℃, placing a piece of silk into each beakers until the mordant is fully dissolved, continuously heating to 80 ℃, stirring for 45min, and washing with deionized water at 40 ℃. And (5) naturally air-drying the sappan wood dyed silk sample, and then filling the sample into a self-sealing bag to be tested.
9) Preparing 4 beakers, pouring 250mL of 1mol/L hydrofluoric acid solution respectively, putting 4 pieces of sample cloth into the 4 beakers respectively, stirring for 20min, slowly pouring 50mL of 5wt% sodium hypochlorite solution under stirring, taking out the sample cloth after 60min, washing with deionized water, and airing.
10 And (3) detecting the isotope of the strontium carbon nitride of the sample by adopting TIMS to the sample to be detected in the steps 1, 3, 4, 5, 7, 8 and 9.
The raw materials and equipment used in the invention are common raw materials and equipment in the field unless specified otherwise; the methods used in the present invention are conventional in the art unless otherwise specified.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (3)
1. The method for removing hematoxylin dye for silk strontium isotope detection is characterized by comprising the following steps of:
1) Placing 30-38 g of massive natural sappan wood in a container, adding 500-1000mL of deionized water, soaking at 20-30 ℃ for 20-40min, drying, pulverizing sappan wood into powder, and filling into a sample bottle for testing;
2) Weighing 250-350mL of deionized water, pouring the deionized water into a sample bottle, and soaking the sample bottle for 6-8 hours at 20-30 ℃;
3) Placing the sample bottle in a constant temperature heating stirrer, heating to 35-45 ℃, and adding 1.5-2.0 g of Na 2 CO 3 Continuously heating to 75-85deg.C, stirring at constant temperature for 50-70min, vacuum filtering, pouring the residue into sample bottle, and collecting filtrate as Sucus Caesalpiniae sappan;
4) Repeating the step 3) twice to obtain two sappan wood juice and three sappan wood juice; finally, drying filter residues, and filling the filter residues into a self-sealing bag to be tested;
5) Uniformly mixing the first sappan juice, the second sappan juice and the third sappan juice to obtain mixed dye liquor, carrying out suction filtration, adjusting the pH of the dye liquor to 6-7 by using acetic acid solution, and taking 40-60mL of dye liquor into a centrifuge tube to be tested;
6) Weighing 20-25 g of blank silk sample, cutting into a plurality of pieces, soaking in a cleaning solution, taking out, cleaning with deionized water, taking a piece of cleaned blank silk sample, naturally air-drying, and filling into a self-sealing bag to be tested;
7) Taking 4 beakers, numbering A, B, C, D, taking 250-300 mL of the dye liquor in the step 5) from each beaker, weighing 1.25-1.5 g of natural iron alum, potassium alum and chromium alum as mordants, and respectively adding the natural iron alum, the potassium alum and the chromium alum into the B, C, D # beakers;
8) Placing the 4 beakers in a constant-temperature heating stirrer, heating while stirring, when the temperature is raised to 35-45 ℃, placing a piece of silk into each beakers until the mordant is fully dissolved, continuously heating to 75-85 ℃, stirring for 40-50min, washing with 35-45 ℃ deionized water, naturally air-drying a sappan-dyed silk sample, and placing the sappan-dyed silk sample into a self-sealing bag for testing;
9) Preparing 4 beakers, respectively pouring 250-300 mL of hydrofluoric acid solution with the concentration of 1mol/L, respectively placing 4 sappan-dyed silk samples into the 4 beakers, stirring, slowly pouring 40-60mL of sodium hypochlorite solution with the concentration of 5wt%, taking out the sappan-dyed silk samples after 55-65 min, washing with deionized water, and airing;
10 And (3) detecting the isotope of the strontium carbon nitride of the oxyhydroxide by using TIMS for the samples to be detected obtained in the steps 1), 3), 4), 5), 7), 8) and 9).
2. The method of claim 1, wherein in step 5), the concentration of the acetic acid solution is 8 to 12wt%.
3. The method according to claim 1, wherein in the step 6), the blank silk sample has a mass of 20-25 g, is cut into 4 pieces, has a size of 20.0cm x 20.0cm, and is soaked for 20-40min with a volume ratio of water to ethanol in a cleaning solution of 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110686873.2A CN113432944B (en) | 2021-06-21 | 2021-06-21 | Method for removing hematoxylin dye for silk strontium isotope detection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110686873.2A CN113432944B (en) | 2021-06-21 | 2021-06-21 | Method for removing hematoxylin dye for silk strontium isotope detection |
Publications (2)
| Publication Number | Publication Date |
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| CN113432944A CN113432944A (en) | 2021-09-24 |
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