CN102455293B - Method for determining trace lead in textile products - Google Patents
Method for determining trace lead in textile products Download PDFInfo
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- CN102455293B CN102455293B CN201110376421.0A CN201110376421A CN102455293B CN 102455293 B CN102455293 B CN 102455293B CN 201110376421 A CN201110376421 A CN 201110376421A CN 102455293 B CN102455293 B CN 102455293B
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Abstract
The invention discloses a method for determining trace lead in textile products, which comprises the following steps of: after a heavy metal Pb in a textile product is extracted by using acidic perspiration, gathering a trace heavy metal Pb in an extracting solution by using nano TiO2; and then, carrying out determination by using an ICP-OES (inductively coupled plasma optical emission spectroscopy) method. Because the content of the heavy metal Pb in the solution subjected to gathering is high, the determination sensitivity is improved, and a determination operation can be performed by using an ICP (inductively coupled plasma) emission spectrum; and in the process of gathering, the salt content in a textile-product extracting solution is reduced, thereby reducing the matrix interference in the process of spectrum determination.
Description
Technical field
The invention belongs to inspection and quarantine field, be specifically related to a kind of method of measuring trace lead in textile products.
Background technology
China is maximum in the world fabric clothing producing country, exported country and country of consumption, and textile industry is the China's export mainstay industry of earning foreign exchange.According to Chinese customs statistics, show, during the 1-11 month in 2007,1606.51 hundred million dollars of China's textile and clothing gross export values, account for 60.28% of national favourable trade balance total value.At present, the Countries of the U.S., Japan, Hong Kong and European Union is the main exporting country of China's textile product, and these countries and regions are conventionally using the safety of textile, sanitary index as weighing one of major criterion of its inherent quality, by promulgating a decree, the form such as compulsory standard, textile has been formulated to multiple Environmental security project demand, only had the product that meets its requirement to be just allowed to enter its market.For this reason; strengthen and accelerate the detection method of poisonous and harmful substance (as heavy metal) in textile and study in existence form (valence state, form); be conducive to improve the detection technique level of China; to ensureing human health and protection of the environment; improve rapidly China's textile ecological standard level; break foreign technology barrier, the development that promotes the ecological textile of China will play a significant role, and tool is of great significance.
Textile, in printing and dyeing and rear arrangement process, is snugness of fit and the colour fastness of raising textile, and textile often will be used various chemical assistants in process, makes residual poisonous and harmful substance in textile, and one of them is exactly poisonous and harmful heavy metallic.These heavy metals have serious cumulative toxicity to human body.In recent years, formulated ecological textile relevant laws and regulations and standard both at home and abroad, strictly limited Pb, Hg, As, Ni, Cu, Co, Cd, Cr, Cr(VI in textile), the content of the heavy metal such as Sb, prohibite substandard product immigration.In China standard GB/T/T 18885-2002 < < ecological textile technical requirement > >, the content of the harmful heavy metal that can extract in textile is also had to clear and definite restriction.
In the world the mensuration of heavy metal in textile is mainly contained: 1). colorimetric analysis 2). atomic absorption spectrophotometry 3). atomic fluorescence spectrum.4). inductively coupled plasma emission spectrography (ICP-OES method).5). inductively coupled plasma mass spectrometry (ICP-MS method).But colorimetric method for determining sexavalent chrome serious interference, sensitivity is not high; Atomic absorption spectrophotometry can not be carried out multielement simultaneous determination, and detection speed is slow; Matrix effect is serious, needs to use matrix modifier, comparatively trouble; And some element determination sensitivity is not high; It is limited that atomic fluorescence spectrum can be surveyed element, can not measure multielement simultaneously; ICP-MS method is due to expensive, and maintenance cost is high, current less employing.Now, because ICP-OES method can be carried out multielement simultaneous determination, and measure when being widely used in textile detection device for multi metallic elements.But because it belongs to the instrument of microanalysis, for trace analysis, sensitivity does not reach requirement, for example, in Pb ion concentration, during lower than 10ng/mL, Accurate Determining has difficulties, insufficient sensitivity.This instrument is for the higher sample of salt (containing a large amount of salinities in acidic sweat) simultaneously, and matrix effect is serious.
In general, due to very low to the heavy metal limit in textile in the world, to testing, bring very large difficulty, current method equipment purchasing total expenses, safeguard that total expenses and personnel's total expenses are all very expensive, be difficult to realize highly sensitive, low-cost, multielement and detect simultaneously, the mensuration new method highly sensitive in the urgent need to setting up, detection speed is fast, cost is low.Yet there are no relevant nano-TiO
2for textile enriched with trace heavy metal Pb, the bibliographical information that then using plasma emission spectrometry is measured.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method of measuring trace lead in textile products.The method is, after the heavy metal lead in textile is extracted with acidic sweat, to adopt nano titanium oxide (TiO
2) trace heavy metal plumbous (Pb) in extracting and enriching liquid, the Pb in extract is concentrated, make its concentration can reach the sensitivity of inductive coupling plasma emission spectrograph.Solved in Pb ion concentration during lower than 10ng/mL, also can adopt inductively coupled plasma emission spectrography (ICP-OES) to measure the problem of the trace Pb in textile, the method can Accurate Determining extract in Pb concentration below 5ng/mL.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A method of measuring trace lead in textile products, the method comprises the following steps:
(1) take acidic sweat as extract, soak textile;
(2) adopt the lead in nano titanium oxide extracting and enriching liquid;
(3) adopt inductively coupled plasma emission spectrography to measure plumbous content.
Further, in step (2), adopt plumbous concrete steps in nano titanium oxide extracting and enriching liquid to be:
A. get the extract 30ml ~ 70mL obtaining in step (1), regulate pH4 ~ 7, add at least 0.03 g nano titanium oxide, shake at least 5min, then static 30min, centrifugal, removes supernatant, obtains nano titanium oxide sediment; Be preferably: add 0.03 g ~ 0.07g nano titanium oxide, concussion 5min ~ 15min;
B. to adding at least concentration of 3ml in described nano titanium oxide sediment, be 0.5 ~ 2mol/L hydrochloric acid, shake at least 5min, then static 30min, centrifugal, obtains supernatant, to be determined.Be preferably: the concentration that adds 3ml ~ 6ml is 0.5 ~ 2mol/L hydrochloric acid concussion 5min ~ 15min;
Further, the formula of described acidic sweat is: in every 1L water, contain L-Histidine 0.5 g, sodium chloride 5 g, two hypophosphite monohydrate sodium dihydrogen 2.2 g.
Further, in step (1), take acidic sweat as extract, the condition of soaking textile is: 37 ℃ are soaked 60min, take out textile, and extract is cooled to room temperature, filter stand-by.
Beneficial effect of the present invention:
(1) the present invention, by the heavy metal lead in textile with after acidic sweat extraction, adopts nano-TiO
2trace heavy metal Pb in extracting and enriching liquid, then measures by ICP-OES method.Because content of beary metal in solution after enrichment is high, improved mensuration sensitivity, can adopt ICP emission spectrum to measure.
(2) use the instrument of microanalysis just can complete trace analysis, saved funds.
(3) in enrichment process, in textile extract, salinity reduces, and the matrix while therefore having reduced spectroscopic assay disturbs.
Below in conjunction with specification drawings and specific embodiments, the invention will be further described, do not limit the present invention in any way.Every any this area of carrying out according to the disclosure of invention is equal to replacement, all belongs to protection scope of the present invention.
Accompanying drawing explanation
Fig. 1 adsorption rate and nanometer Ti O
2the graph of a relation of consumption;
The graph of a relation of Fig. 2 adsorption rate and adsorbing medium acidity;
The graph of a relation of Fig. 3 measured value and the time of parsing;
The graph of a relation of Fig. 4 measured value and concentration of hydrochloric acid.
specific embodiment mode
embodiment 1
1 instrument and reagent
Prodigy XP inductively coupled plasma atomic emission spectrometer (Leeman company), its condition of work: power is 1.2 KW, atomization gas pressure 28 psi, assisted gas flow 0.1 LPM, cooling gas flow: 20 LPM; Pump speed: 1.5 mL/min, Pb detects wavelength 220.353 nm.
Pb standard solution is provided by State center for standard matter.
It is pure or analyze pure that the various conventional reagent of experiment use is top grade.
Experimental water is 18.2 M Ω cm ultrapure waters.
Nanometer Ti O
2(mean grain size≤25 nm) is purchased from Hangzhou Wan Jing new material company limited.
The preparation of acidic sweat: take L-Histidine 0.5g, sodium chloride 5g, two hypophosphite monohydrate sodium dihydrogen 2.2 g dissolve in beaker, are transferred in 1L volumetric flask.
2 experimental techniques
2.1 nano-TiO
2process
By nano-TiO
2be put in beaker, the nitric acid dousing 30min with 5mol/L, is washed till neutrality with ultrapure water, after oven dry, keeps in Dark Place.
2.2 sample pre-treatments
Cloth specimen is shredded to 5mm X 5mm, mix, take 4.00g sample, be placed in tool plug Erlenmeyer flask.Add 80mL acidic sweat, fiber is fully soaked, put into 37 ℃ of water bath with thermostatic control oscillators 60min that vibrates, after taking-up, the standing room temperature that is cooled to, filters, and filtrate (extract) is tested for concentration and separation.
2.3 experimental technique
In 50mL tool plug centrifuge tube, add the extract in 30mL step 2.2, then add a certain amount of nano-TiO
2, mechanical oscillation, standing 30min, the centrifugal 15min of 5300r/min, removes supernatant liquor.
Nano-TiO after centrifuging
2in sediment, accurately add a certain amount of certain density HCl, mechanical oscillation again, standing 30min, the centrifugal 15min of 5300r/min, gets supernatant and measures wherein plumbous content with ICP-OES.
3. the selection of condition
3.1 adsorption conditions
3.1.1 nano-TiO
2consumption
Respectively at adding 0.01,0.02,0.03,0.04,0.05 in six centrifuge tubes, the nano titanium oxide of 0.07g, the experimental technique by 2.3 operates, and the results are shown in Figure 1.Show that the consumption of nano material titania is more than 0.03g, but consider experimental cost, too much add nano titanium oxide without any meaning, so the consumption of nano titanium oxide is preferably 0.03g ~ 0.07g.
3.1.2 adsorption time:
According to 2.3 experimental techniques, operate, vibrate respectively 5,10,15,20,25, standing 30min after 30min, the 5min that shows to vibrate can obtain better absorption above, but considers the control to whole experimental period, is preferably concussion 5-30min.
3.1.3 adsorb acidity
In 6 centrifuge tubes, add respectively a certain amount of acidic sweat, regulate pH value to be respectively 1,2,3,4,5.5,7, then according to 2.3 experimental techniques, operate, the results are shown in Figure 2.Show that pH scope is 4～7, absorption better.
3.2 desorption condition
3.2.1 desorption time
By the nano-TiO after centrifuging
2sediment adds a certain amount of 0.5mol/mL HCl, vibrates respectively 5,10,15,25, and 30 min, then operate according to 2.3 experimental techniques, the results are shown in Figure 3.The 5min that shows to vibrate can obtain better desorption effect above, but considers the control to whole experimental period, is preferably concussion 5-30min.
3.2.2 desorb acidity
The centrifugal sediment obtaining is added respectively to 6 mL0.05, and 0.1,0.5,1,1.5,2mol/mL HCl, operates by 2.3 experimental techniques, and Pb content in centrifugal rear mensuration supernatant, the results are shown in Figure 4.Show that concentration of hydrochloric acid is better in 0.5 ~ 2mol/L desorb.
3.3.3 hydrochloric acid consumption
By add respectively the 0.5mol/mL HCl of 3,4,5,6 mL in nano material absorption, the centrifugal sediment obtaining, by 2.3 experimental procedures, operate, the results are shown in Table 1.Show that hydrochloric acid consumption is more than 3mL, but consider experimental cost, too much add hydrochloric acid without any meaning, so concentration is that the consumption of 0.5mol/mL HCl is preferably 3 ~ 6ml.
Table 1 hydrochloric acid consumption
| 0.5N HCl consumption/mL | Addition/ug | Measured value/ug | The recovery/% |
| 3 | 0.3 | 0.2976 | 99.2 |
| 4 | 0.3 | 0.3036 | 101.2 |
| 5 | 0.3 | 0.301 | 100.3 |
| 6 | 0.3 | 0.3012 | 100.4 |
4. detection lower bound, the recovery and the precision of method
Respectively at adding nano titanium oxide in 7 centrifuge tubes, then add respectively 0.3ugPb standard solution, a certain amount of acid acidic sweat, making Pb concentration is 5ng/mL, by 2.3 experimental procedures, operates, and the results are shown in Table 2.This result shows: when the concentration of Pb is low to moderate 5ng/mL, the recovery of the method is between 87% ~ 101%, and relative standard deviation is below 6%.Explanation can Accurate Determining be low to moderate the Pb of 5ng/mL.
The recovery of table 2 method and precision
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (1)
1. a method of measuring trace lead in textile products, is characterized in that, the method comprises the following steps:
(1) nano-TiO
2process
By nano-TiO
2be put in beaker, the nitric acid dousing 30min with 5mol/L, is washed till neutrality with ultrapure water, after oven dry, keeps in Dark Place;
(2) sample pre-treatments
Cloth specimen is shredded to 5mm * 5mm, mix, take 4.00g sample, be placed in tool plug Erlenmeyer flask, add 80mL acidic sweat, fiber is fully soaked, put into 37 ℃ of water bath with thermostatic control oscillators 60min that vibrates, after taking-up, the standing room temperature that is cooled to, filter, filtrate is that extract is for concentration and separation;
(3) in 50mL tool plug centrifuge tube, add the extract in 30mL step (2), regulate pH4～7, then add 0.03g～0.07g nano-TiO
2, mechanical oscillation 5min～30min, standing 30min, the centrifugal 15min of 5300r/min, removes supernatant liquor;
Nano-TiO after centrifuging
2the hydrochloric acid that the concentration that accurately adds 3～6ml in sediment is 0.5～2mol/L, mechanical oscillation 5min～30min again, standing 30min, the centrifugal 15min of 5300r/min, gets inductively coupled plasma emission spectrographic determination plumbous content wherein for supernatant;
And, the preparation of described acidic sweat: take L-Histidine 0.5g, sodium chloride 5g, two hypophosphite monohydrate sodium dihydrogen 2.2g dissolve in beaker, are transferred in 1L volumetric flask.
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| CN102455293B true CN102455293B (en) | 2014-07-23 |
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| CN103389317B (en) * | 2013-07-28 | 2015-11-25 | 浙江出入境检验检疫局检验检疫技术中心 | A kind of Analysis of Heavy Metal method in textile |
| CN103728170B (en) * | 2014-01-07 | 2015-10-28 | 中华人民共和国北京出入境检验检疫局 | Proficiency testing sample of and chrome determination plumbous for textile extractable heavy metal and preparation method thereof |
| CN104807727B (en) * | 2014-12-22 | 2018-08-28 | 中华人民共和国象山出入境检验检疫局 | The detection method of benzophenone compound the amount of migration in a kind of textile |
| CN106872454A (en) * | 2017-01-13 | 2017-06-20 | 上海市质量监督检验技术研究院 | The screening technique of total lead content in a kind of textile |
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| CN101811024A (en) * | 2010-04-02 | 2010-08-25 | 同济大学 | Preparation of solid phase extractant for enriching lead ions and application method thereof |
| CN101914059B (en) * | 2010-08-18 | 2012-12-19 | 云南烟草科学研究院 | Analytical reagent for detecting trace lead as well as preparation method and application thereof |
| CN101975771A (en) * | 2010-09-14 | 2011-02-16 | 常熟出入境检验检疫局综合技术服务中心 | Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder |
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