CN105334096A - Method for performing strontium element enrichment on silk fabric cultural relics - Google Patents

Abstract

The invention provides a method for performing strontium element enrichment on silk fabric cultural relics. The method comprises the following steps that 1, an appropriate quantity of silk fabrics are taken and soaked in 7 ml-10 ml of a hydrofluoric acid solution HF (aq) with the mass percent of 20%, and ultrasonic treatment is performed for 1-2 h at room temperature; 2, the undissolved silk fabrics are taken out and flushed with deionized water for twice to obtain the remaining silk fabrics; 3, 10 ml-20 ml of an HNO3 solution with the mass percent of 30% and 10 ml-20 ml of a hydrogen peroxide solution with the mass percent of 30% are taken and fully mixed to obtain a solution A; 4, the silk fabric cultural relics obtained in the step 2 are dissolved in the solution A, and static standing is performed at the constant temperature of 30 DEG C for 15 min-1 h to obtain a solution B; 5, the solution B is evaporated to be dry on a heating plate with the temperature of 80 DEG C to obtain a solid C; 6, a few of the solid C is taken and dissolved in an HNO3 solution with the concentration of 3 mol/L to obtain a solution D; 7, separation and enrichment are performed on the solution D through 50-100-mesh SrSpecTM resin quartz columns, and then the resin columns are eluted by taking deionized water as eluent to obtain a solution E. The method has the advantages of being high in sensitivity and specificity and the like.

Description

A kind of method of carrying out strontium element enrichment for silk fabric cultural relics

Technical field

The present invention relates to a kind of strontium element enrichment method, particularly relate to a kind of method of carrying out strontium element enrichment for silk fabric cultural relics.

Background technology

Silk is first historically worldwide commodity, and the source of silk relics is the direction of the nearly Controlling research for over 100 years more than a hundred years of historian and archaeologist always.Although pattern, style and weaving technology etc. were once the important method judging silk area of origin, in view of the blending of civilization converges mutually, these method neither ones can give conclusive evidence for the source of silk.

At present, utilizing strontium stable isotope to carry out tracing to the source of the silk goods place of production is carry out textile historical relic to trace to the source method system more accurately, and the science that also surely belongs to carries out the developing direction that textile historical relic isotope technology is traced to the source.But content of strontium is very little in silk fabric cultural relics, be difficult to the numerical value detecting that it is determined.Therefore, before carrying out strontium element detection to silk fabric cultural relics, it is very necessary for carrying out enrichment targetedly.

Summary of the invention

The object of the invention is to provide a kind of method of carrying out strontium element enrichment for silk fabric cultural relics for above-mentioned Problems existing.

The technical solution adopted in the present invention is: a kind of method of carrying out strontium element enrichment for silk fabric cultural relics, comprises the steps:

1) getting appropriate silk goods is immersed in the hydrofluoric acid solution HF (aq) of 7ml ~ 10ml mass percent 20%, at room temperature ultrasonic process 1 ~ 2h;

2) above-mentioned not molten silk goods are taken out, with deionized water rinsing 2 times, obtain remaining silk goods;

3) hydrogen peroxide solution of the HNO3 solution and 10 ~ 20ml mass percent 30% of getting 10 ~ 20ml mass percent 30% is fully mixed to get solution A;

4) by step 2) silk fabric cultural relics that obtains is dissolved in solution A, and under constant temperature 30 DEG C of conditions, leave standstill 15min ~ 1h, obtain solution B;

5) solution B evaporate to dryness is obtained solid C;

6) get a little solid C to be dissolved in the HNO3 solution of 3mol/L, obtain solution D;

7) solution D is passed through 50 ~ 100 object SrSpec ^tMresin quartz column carries out separation and concentration, then is that eluent carries out wash-out to resin column with deionized water, obtains solution E.

Step 5) in, solution B evaporate to dryness on the heating plate of 80 DEG C.

Beneficial effect of the present invention is: highly sensitive, high specificity, is to detect more efficient a kind of enrichment method for content of strontium in silk fabric cultural relics.

Embodiment

Embodiment 1

Carry out a method for strontium element enrichment for silk fabric cultural relics, comprise the steps:

1) getting appropriate silk goods is immersed in the hydrofluoric acid solution HF (aq) of 7ml mass percent 20%, at room temperature ultrasonic process 1h;

2) above-mentioned not molten silk goods are taken out, with deionized water rinsing 2 times, obtain remaining silk goods;

3) hydrogen peroxide solution of the HNO3 solution and 20ml mass percent 30% of getting 10ml mass percent 30% is fully mixed to get solution A;

4) by step 2) silk fabric cultural relics that obtains is dissolved in solution A, and under constant temperature 30 DEG C of conditions, leave standstill 15min, obtain solution B;

5) heating plate evaporate to dryness solution B being placed on 80 DEG C obtains solid C;

6) getting a little solid C is dissolved in the HNO3 of 3mol/L, obtains solution D;

7) by solution D by being mounted with 50 object SrSpec ^tMresin is concentrated clean, then uses deionized water wash-out, obtains solution E; In this process, organic compound basically by resin, but also has and has been bonded on resin column on a small quantity, and with in the process of washed with de-ionized water, a small amount of organic compound is retained on resin, because initial white resin becomes light brown.

Embodiment 2

Carry out a method for strontium element enrichment for silk fabric cultural relics, comprise the steps:

1) getting appropriate silk goods is immersed in the hydrofluoric acid solution HF (aq) of 10ml mass percent 20%, at room temperature ultrasonic process 2h;

2) above-mentioned not molten silk goods are taken out, with deionized water rinsing 2 times, obtain remaining silk goods;

3) hydrogen peroxide solution of the HNO3 solution and 10ml mass percent 30% of getting 20ml mass percent 30% is fully mixed to get solution A;

4) by step 2) silk fabric cultural relics that obtains is dissolved in solution A, and under constant temperature 30 DEG C of conditions, leave standstill 1h, obtain solution B;

5) heating plate evaporate to dryness solution B being placed on 80 DEG C obtains solid C;

6) getting a little solid C is dissolved in the HNO3 of 3mol/L, obtains solution D;

7) solution D is passed through 100 object SrSpec ^tMresin quartz column carries out separation and concentration, then is that eluent carries out wash-out to resin column with deionized water, obtains solution E; In this process, organic compound basically by resin, but also has and has been bonded on resin column on a small quantity, and with in the process of washed with de-ionized water, a small amount of organic compound is retained on resin, because initial white resin becomes light brown.

Embodiment 3

Carry out a method for strontium element enrichment for silk fabric cultural relics, comprise the steps:

1) getting appropriate silk goods is immersed in the hydrofluoric acid solution HF (aq) of 8ml mass percent 20%, at room temperature ultrasonic process 1.5h;

2) above-mentioned not molten silk goods are taken out, with deionized water rinsing 2 times, obtain remaining silk goods;

3) hydrogen peroxide solution of the HNO3 solution and 15ml mass percent 30% of getting 15ml mass percent 30% is fully mixed to get solution A;

4) by step 2) silk fabric cultural relics that obtains is dissolved in solution A, and under constant temperature 30 DEG C of conditions, leave standstill 40min, obtain solution B;

5) heating plate evaporate to dryness solution B being placed on 80 DEG C obtains solid C;

6) getting a little solid C is dissolved in the HNO3 of 3mol/L, obtains solution D;

7) solution D is passed through 80 object SrSpec ^tMresin quartz column carries out separation and concentration, then is that eluent carries out wash-out to resin column with deionized water, obtains solution E; In this process, organic compound basically by resin, but also has and has been bonded on resin column on a small quantity, and with in the process of washed with de-ionized water, a small amount of organic compound is retained on resin, because initial white resin becomes light brown.

Claims (2)

1. carry out a method for strontium element enrichment for silk fabric cultural relics, it is characterized in that comprising the steps:

1) getting appropriate silk goods is immersed in the hydrofluoric acid solution HF (aq) of 7ml ~ 10ml mass percent 20%, at room temperature ultrasonic process 1 ~ 2h;

2) above-mentioned not molten silk goods are taken out, with deionized water rinsing 2 times, obtain remaining silk goods;

3) hydrogen peroxide solution of the HNO3 solution and 10 ~ 20ml mass percent 30% of getting 10 ~ 20ml mass percent 30% is fully mixed to get solution A;

4) by step 2) silk fabric cultural relics that obtains is dissolved in solution A, and under constant temperature 30 DEG C of conditions, leave standstill 15min ~ 1h, obtain solution B;

5) solution B evaporate to dryness is obtained solid C;

6) get a little solid C to be dissolved in the HNO3 solution of 3mol/L, obtain solution D;

7) solution D is passed through 50 ~ 100 object SrSpec ^tMresin quartz column carries out separation and concentration, then is that eluent carries out wash-out to resin column with deionized water, obtains solution E.

2. method of carrying out strontium element enrichment for silk fabric cultural relics according to claim 1, is characterized in that: step 5) in, solution B evaporate to dryness on the heating plate of 80 DEG C.