CN104236966A - Method for detecting content of extractable arsenic in textile - Google Patents
Method for detecting content of extractable arsenic in textile Download PDFInfo
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- CN104236966A CN104236966A CN201310246495.1A CN201310246495A CN104236966A CN 104236966 A CN104236966 A CN 104236966A CN 201310246495 A CN201310246495 A CN 201310246495A CN 104236966 A CN104236966 A CN 104236966A
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Abstract
The invention relates to a method for detecting total arsenic in a textile. The method comprises the steps of performing hydrogenation on a sample after arsenic (V) in an extracted sample obtained by treating the textile is reduced to arsenic (III), detecting a generated hydride by an inductively coupled plasma emission spectrometer, and measuring the content of trace arsenic in the textile. Treatment on the textile comprises: cutting the textile to be detected, performing extraction by an acidic extraction solution, separating so as to obtain the extracted sample, adding a reducing agent which is selected from one or more of hydroxy lamine hydrochloride, ascorbic acid, potassium iodide, thiourea, potassium ferrocyanide and sodium sulfite, mixing the reduced sample with a hydrochloric acid solution to obtain a mixture, and then mixing the mixture with a sodium borohydride solution to enable the arsenic (III) in the sample to generate gaseous arsenic hydride AsH3; and introducing the hydride AsH3 into an inductively coupled plasma rectangular pipe, atomizing, exciting arsenic elements under the temperature of about 6,000-7,000 DEG C, and quantitatively analyzing the content of the arsenic of the sample.
Description
Technical field
The present invention relates to the detection method of arsenic in a kind of textile, be specifically related to the detection method that can extract micro amount of arsenic in a kind of textile, after the arsenic (V) existed in extraction sample is reduced to arsenic (III), after hydrogenation is carried out to sample, carry out hydride generation inductive coupling plasma emission spectrum (ICP-AES) method and detect micro amount of arsenic content, the i.e. method of total arsenic content in textile.
Background technology
Arsenic is a kind of harmful element, and usually exist with pentavalent arsenic and trivalent arsenic, wherein the toxicity of trivalent is larger.The compound of arsenic is applied to agricultural, is used as pesticide, removes seed agent and poison etc.The approach that other natures touch arsenic element comprises the weathering of volcanic debris, arsenic-containing ores and ore and is dissolved by underground water.Arsenic also can be present in food, water body, soil and air.Arsenic can by all plant absorption, but easier enrichment in pot-herb, rice, apple and grape juice and marine product.Strict limitation requirement is had to arsenic in Oeko-Tex Standard.As the content requirement of arsenic can be extracted lower than 0.2mg/kg in infant article.There is following defect in the current existing method of inspection:
1, ICP-AES: because in textile acid extract sample used, salt content is higher, causes background interference large, have impact on the detectability of mensuration.
2, arsenic, mercury atom fluorescence spectrophotometry: in mensuration, atomization temperature is low, and atomization efficiency is not high, and the working curve range of linearity is narrow, poor stability, and detectability is also poor.
3, chemical determination arsenic often adopts separated-Photometric Determination and extracting n-butyl alcohol-arsenic bismuth Photometric Determination, carrier precipitation-Photometric Determination antimony amount and peacock green-benzene Extraction-Photometric Determination of Antimony amount, these method complex operations, and be harmful to operating personnel's health, and detectability is not high yet.
Summary of the invention
In order to overcome deficiency of the prior art, the invention provides a kind of detection method that can extract micro amount of arsenic for textile, after the arsenic (V) existed in extraction sample is reduced to arsenic (III) by the present invention, adopt in hydride generation-inductive coupling plasma emission spectrum method joint-detection textile and can extract micro-total arsenic content, overcome in above detection method not enough, eliminate loaded down with trivial details lock out operation, improve the sensitivity of mensuration, detect limit for height, easy and simple to handle, quick, analysis result accurately and reliably, can meet the requirement that textile measures arsenic.
To achieve these goals, following technical scheme is adopted:
The detection method of micro amount of arsenic in a kind of textile, textile is extracted, after the arsenic (V) existed in extraction sample is reduced to arsenic (III), after hydrogenation is carried out to sample, measure by hydride generation-inductive coupling plasma emission spectrum method, described inspection comprises the checking procedure of test condition selection, sample preparation, interference elimination, working curve linear relationship, detection limit, relative standard deviation.
Micro amount of arsenic detection method in described textile, instrument is: SPECTRO CIROS
cCD, German Spike instrument company.
The detection method of micro amount of arsenic in described textile, experimental program is; Textile samples to be measured is cut out, is cut into 5 × 5mm, extract with extract, liquid extraction liquid is acid, can be 80ml acidic sweat, after separation, add reductive agent, after the arsenic (V) existed in extraction sample is reduced to arsenic (III), mix with hydrochloric acid solution, then mix with sodium borohydride solution, make arsenic (III) generate the AsH3 of gaseous state, be carrier gas with high-purity argon gas, by AsH
3be incorporated in inductively coupled plasma quarter bend, at high temperature, temperature about 6000 ~ 7000 DEG C, arsenic element atomization excited, launch characteristic spectral line, line strength is directly proportional to the concentration of arsenic element in test solution to be measured; Accordingly can arsenic amount in quantitative test test solution.
With reductive agent, arsenic (V) is reduced to arsenic (III), reductive agent used is selected from oxammonium hydrochloride, ascorbic acid, potassium iodide, thiocarbamide, potassium ferrocyanide, one or more in sodium sulphite.Preferred potassium iodide-ascorbic acid, thiourea and ascorbic acid, sodium sulphite.
Micro amount of arsenic detection method in described textile, in test solution, the atomization process of arsenic is:
BH
4 -+H
++3H
2O→H
3BO
3+8H
2As
3++ 8H → 2AsH
3+ H
2↑ (excessive)
2AsH
3→2As+3H
2↑
Micro amount of arsenic detection method in described textile, actual conditions:
One, experiment condition:
The choice of spectrum of A, mensuration: As189.042nm or As193.759nm, preferably measures under the wavelength of As189.042nm.
B, instrument power, cooling gas flow, the selection of assisted gas flow and carrier gas flux: preferably plasma generation power is 1500W, cooling gas flow 14.00L/min, assisted gas flow 1.20L/min, carrier gas flux 0.40L/min.
The selection of C, concentration of hydrochloric acid:
Mix with liquid to be measured with variable concentrations hydrochloric acid, mix with the sodium borohydride solution of fixed concentration again, measure the intensity of emission spectra of arsenic in liquid to be measured, the concentration of hydrochloric acid solution that test selection measures arsenic is: 1.0% ~ 4.0% (volume), preferably 3% (volume).
The selection of D, sodium borohydride concentration:
Fixing concentration of hydrochloric acid, make it to mix with liquid to be measured, then mix with the sodium borohydride solution of variable concentrations, measure the intensity of emission spectra of arsenic, the sodium borohydride solution concentration that test selection measures arsenic is: 1.0% ~ 4.0% (weight), preferably 1.5% (weight).
The selection of E, reductive agent and consumption:
The valence state of the acidic sweat extraction arsenic in sample of textile exists with the mixed form of (V) valency with (III) valency, because arsenic (V) is difficult to directly generate arsenic hydride with sodium borohydride.Only have and first wherein will be reduced into arsenic (III) by arsenic (V), the whole arsenic in extraction sample and sodium borohydride just can be made to generate hydride of arsenic.With reductive agent, arsenic (V) is reduced to arsenic (III), reductive agent used is selected from oxammonium hydrochloride, ascorbic acid, potassium iodide, thiocarbamide, potassium ferrocyanide, one or more in sodium sulphite.Preferred potassium iodide-the ascorbic acid of reductive agent, thiourea and ascorbic acid, sodium sulphite.The element such as chromium, copper, nickel, cobalt, lead, bismuth existed due to the element such as sodium, phosphorus and the trace of a large amount of existence in textile acidic sweat extraction sample matrices is noiseless to reduction reaction, the present invention preferably makes the reductive agent of arsenic with sodium sulfite solution, be characterized in low price, reduction mechanism is simply clear, other factors are little on reduction reaction impact, and reduzate is simple.
Two, sample preparation:
Preparation acidic sweat: the L-Histidine hydrochloride secondary deionized water of getting 0.5g is dissolved in 100mL small beaker, 2.2g sodium dihydrogen phosphate dihydrate is added in small beaker, finally add 5g sodium chloride and make its mixed dissolution, solution in small beaker is transferred in 1L volumetric flask, use secondary deionized water constant volume, be 5.5 by the NaOH adjust ph of 0.1mol/L, namely obtain required acidic sweat.
By textile cutting, be cut into 5 × 5mm size, take 4.0 grams of samples in 150ml tool plug conical flask, add 80ml acidic sweat, in 37 ± 2 DEG C of shaking tables 1 hour, filter with glass sand core funnel, obtain extraction sample, to be measured.
Take 2.0g sodium sulphite, add secondary deionized water and be about after 600mL dissolves, add secondary deionized water constant volume to 1000mL volumetric flask, and must 0.2% (weight) sodium sulphite reducing solution.In like manner can compound concentration be 1%, 2%, 5% and 10% sodium sulfite solution.
Take 2.0g thiocarbamide and 2.0g ascorbic acid respectively, add secondary deionized water and be about after 600mL dissolves, add secondary deionized water constant volume to 1000mL volumetric flask, and must 0.2% (weight) thiourea and ascorbic acid reducing solution.In like manner can compound concentration be 1%, 2%, 5% and 10% thiourea and ascorbic acid solution.
The reduction of extraction sample: get 5ml with transfer pipet and extract sample, add isopyknic reducing solution, add the 0.1mol/L hcl acidifying of 2.0ml.To be measured.
Three, the Interference and Elimination of coexistence elements
Coexistence elements in extraction sample have sodium, phosphorus, and the chromium of trace, copper, nickel, cobalt, lead, bismuth etc., these coexistence elements all do not participate in hydrogenation, also gas would not be become, quarter bend Atom can not be entered, therefore can not produce the corresponding spectral line of emission, greatly reduce the background interference of mensuration, improve the detectability of detection and the sensitivity of mensuration.
Four, working curve
Take acidic sweat as matrix, compound concentration is 0.010,0.050 respectively, the arsenic standard solution of 0.10,0.20mg/L, measures the intensity of emission spectra of arsenic under the instrument condition of work selected and the condition generating hydride, drawing curve, line linearity of going forward side by side returns and calculates.Measure the range of linearity of arsenic.
Five, detection limit test
Carry out 10 METHOD FOR CONTINUOUS DETERMINATION to the blank sample of extract, the standard deviation S D mean value measured with 10 times takes advantage of 3 to obtain detection limit.
Six, relative standard deviation:
Under optional test condition, carry out 10 replications, the relative standard deviation of method to arsenic with for the standard solution of 0.1mg/L.
Owing to taking technical scheme as above, the present invention has following superiority:
Of the present invention for micro amount of arsenic detection method in textile, when arsenic (V) being reduced into arsenic (III) with reductive agent, be preferably that arsenic (V) is reduced to arsenic (III) by reductive agent with thiourea and ascorbic acid, sodium sulfite solution, most preferably sodium sulphite, be characterized in low price, reduction mechanism is simply clear, and other factors are little on reduction reaction impact, and reduzate is simple.By adopting micro amount of arsenic content in hydride generation-inductive coupling plasma emission spectrum method joint-detection textile, there is Matrix effects little, background equipotent concentration (BEC) is low, the working curve range of linearity (L.R) is wide, highly sensitive, good stability, the advantages such as easy and simple to handle, detection speed is fast, analysis result accurately and reliably, can meet in textile the requirement measuring arsenic.
Embodiment
In textile of the present invention, hydride of arsenic generation-inductive coupling method plasma emission spectrum measures the condition of work adopted and is:
Spectral line: As189.042nm; Plasma generation power is 1500W, cooling gas flow 14.00L/min, assisted gas flow 1.20L/min, carrier gas flux 0.40L/min; Full spectra measurement; 120 seconds pre-flush time, multiplicity is 3; Metering system is working curve method; Concentration of hydrochloric acid solution is: 1.0% ~ 4.0% (volume), and sodium borohydride solution concentration is: 1.0% ~ 3.0% weight.
The instrument used is: SPECTRO CIROSCCD, German Spike instrument company.
This test water is secondary deionized water.
Carry out experimental implementation meeting under above-mentioned condition of work.
Embodiment 1:
Acidic sweat is matrix, compound concentration is 0.010,0.050,0.10, the arsenic standard solution of 0.20mg/L, under the condition of work that instrument is selected, at the sodium borohydride solution of 1.5% weight, concentration of hydrochloric acid is under the hydride occurrence condition of 1.0% ~ 4.0% (volume), makes emissive porwer-concentration working curve.
Table 1: the selection of concentration of hydrochloric acid solution (volume)
From table 1: when concentration of hydrochloric acid solution is 3.0%, background equipotent concentration is minimum, namely background interference is minimum, and detectability is minimum, working curve linearly best, and slope of a curve is maximum, and namely detection sensitivity is the highest.
Embodiment 2:
Acidic sweat is matrix, and compound concentration is 0.010,0.050, the arsenic standard solution of 0.10,0.20mg/L, under the condition of work that instrument is selected, concentration of hydrochloric acid is 3.0%, and sodium borohydride solution concentration is: 1.0% ~ 3.0%, draws emissive porwer-concentration working curve.
Table 2: the selection of sodium borohydride solution concentration (weight)
From table 2: when sodium borohydride solution concentration is 3.0%, background equipotent concentration is minimum, and namely background interference is minimum, and detectability is minimum, working curve linearly best, slope of a curve is maximum, and namely detection sensitivity is the highest.
Embodiment 3:
Take about 4.0g 5 × 5mm size cloth specimen in 150ml tool plug conical flask, add 80ml acidic sweat and extract 1 hour in 37 ± 2 DEG C of shaking tables, filter with glass sand core funnel, obtain extraction sample.Acidic sweat is matrix, compound concentration is 0.010,0.050,0.10, the arsenic standard solution of 0.20mg/L, under the condition of work that instrument is selected, at the sodium borohydride solution of 1.5% (weight), concentration of hydrochloric acid is curve of working under the hydride occurrence condition of 3.0% (volume), 0.0030mg/L is added respectively in extraction sample, 0.0050mg/L, 0.0010mg/L arsenic (V) standard solution, reduces with the sodium sulfite solution of 2% weight.Get 5ml and extract sample, add isopyknic reducing solution, add the 0.1mol/L hcl acidifying of 2.0ml.Measuring recovery of standard addition is 89.0% ~ 101.0%.Illustrate that accuracy of measurement is higher under this measuring condition, meet the mensuration requirement of trace materials.
Embodiment 4:
Take about 4.0g 5 × 5mm size cloth specimen in 150ml tool plug conical flask, add 80ml acidic sweat and extract 1 hour in 37 ± 2 DEG C of shaking tables, filter with glass sand core funnel, obtain extraction sample.Acidic sweat is matrix, compound concentration is 0.010,0.050,0.10, the arsenic standard solution of 0.20mg/L, under the condition of work that instrument is selected, at the sodium borohydride solution of 1.5% (weight), concentration of hydrochloric acid is curve of working under the hydride occurrence condition of 3.0% (volume), 0.0030mg/L is added respectively in extraction sample, 0.0050mg/L, 0.0010mg/L arsenic (V) standard solution, with the thiourea and ascorbic acid solution reduction of 5% weight.Get 5ml and extract sample, add isopyknic reducing solution, add the 0.1mol/L hcl acidifying of 2.0ml.Measuring recovery of standard addition is 90.0% ~ 104.0%.Illustrate that accuracy of measurement is higher under this measuring condition, meet the mensuration requirement of trace materials.
Claims (10)
1. the detection method of arsenic in a textile, sample is extracted with after extract process textile, reductive agent is added in extraction sample, hydrogenation is carried out to the sample after reduction, the hydride Inductively coupled plasma optical emission spectrometer generated detects, and records the content of micro amount of arsenic in textile.
2. method according to claim 1, process textile comprises cuts out textile to be measured, extract with acid extract liquid, extraction sample is obtained after being separated, arsenic in sample (V) will be extracted and be reduced to arsenic (III), sample after reduction mixes with hydrochloric acid solution, mix with sodium borohydride solution again, the arsenic in sample (III) is made to generate the arsenic hydride of gaseous state, wherein reductive agent is selected from oxammonium hydrochloride, ascorbic acid, potassium iodide, thiocarbamide, potassium ferrocyanide, one or more in sodium sulphite.
3. method according to claim 2, cuts out textile to be measured and is cut into 5 × 5mm, and acid extract liquid is acidic sweat, and reductive agent is the thiourea and ascorbic acid solution of 5% weight.
4. method according to claim 2, preferred reductive agent is the sodium sulphite of 2% weight.
5. method according to claim 4, the preparation of acidic sweat: the L-Histidine hydrochloride secondary deionized water of getting 0.5g is dissolved in 100mL small beaker, 2.2g sodium dihydrogen phosphate dihydrate is added in small beaker, finally add 5g sodium chloride and make its mixed dissolution, solution in small beaker is transferred in 1L volumetric flask, using secondary deionized water constant volume, is 5.5 by the NaOH adjust ph of 0.1mol/L, namely obtains required acidic sweat.
6. method according to claim 2, concentration of hydrochloric acid solution is 1.0% ~ 4.0% (volume), and sodium borohydride solution concentration is 1.0% ~ 4.0% (weight).
7. method according to claim 2, preferred salt acid solutions is 3.0% (volume), and sodium borohydride solution concentration is 1.5% (weight).
8. the method described in claim 1-7, Inductively coupled plasma optical emission spectrometer device is the SPECTRO CIROS of German Spike instrument company
cCDtake high-purity argon gas as carrier gas, the choice of spectrum measured: measure under the wavelength of As189.042nm or As193.759nm, hydride is incorporated in inductively coupled plasma quarter bend, temperature about 6000 ~ 7000 DEG C, arsenic element atomization is excited, arsenic (III) content in quantitative test sample.
9. the method that one of claim 1-8 is described, preferred plasma generation power is 1500W, spectral line at As189.042nm, cooling gas flow 14.00L/min, assisted gas flow 1.20L/min, carrier gas flux 0.40L/min.
10. the method that one of claim 1-8 is described, extracts in sample at 5ml, adds isopyknic reductant solution, add the 0.1mol/L hcl acidifying of 2.0ml.
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Cited By (5)
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| CN107860851A (en) * | 2017-11-06 | 2018-03-30 | 山东省计量科学研究院 | A kind of standard substance for trivalent arsenic Elemental Speciation Analysis and preparation method thereof |
| CN110455784A (en) * | 2019-08-30 | 2019-11-15 | 楚雄滇中有色金属有限责任公司 | A kind of method of arsenic content in sulfuric acid |
| CN112813647A (en) * | 2019-11-18 | 2021-05-18 | 海尔智家股份有限公司 | Method for acquiring salinity information on clothes and electronic equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105223179A (en) * | 2015-10-23 | 2016-01-06 | 中华人民共和国莆田出入境检验检疫局 | A kind of method of arsenic, antimony and the mercury that can extract in AFS DETERMINATION leather |
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| CN110455784A (en) * | 2019-08-30 | 2019-11-15 | 楚雄滇中有色金属有限责任公司 | A kind of method of arsenic content in sulfuric acid |
| CN112813647A (en) * | 2019-11-18 | 2021-05-18 | 海尔智家股份有限公司 | Method for acquiring salinity information on clothes and electronic equipment |
| CN112813647B (en) * | 2019-11-18 | 2024-02-27 | 重庆海尔滚筒洗衣机有限公司 | Method for acquiring information of salinity on clothes and electronic equipment |
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