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首页> 外文期刊>The Journal of the American Leather Chemists Association >SAMPLE PREPARATION PROCEDURES FOR DETERMINATION OF Cr_2O_3 IN LEATHER SAMPLES USING ICP-AES AND AAS
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SAMPLE PREPARATION PROCEDURES FOR DETERMINATION OF Cr_2O_3 IN LEATHER SAMPLES USING ICP-AES AND AAS

机译:ICP-AES和AAS测定皮革样品中Cr_2O_3的样品制备方法。

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摘要

Three different sample preparation procedures were applied to leather samples, representing four different steps of the tanning process namely, after the tanning step (wet blue), after the retanning step (crust), after normal finishing and after a silicon finishing process. The sample preparation procedures are the conventional procedure in which the samples are fused at 800℃ with a mixture of Na_2CO_3, K_2CO_3 and borax followed by dissolving in boiling water and filtering. The other two suggested procedures are an ashing/fusion procedure in which the leather sample is ashed at 1000℃ followed by an alkali fusion step with NaOH, Na_2O_2 and Na_2CO_3 while in the second procedure the leather sample is refluxed with concentrated HNO_3. Both procedures lead to complete dissolution of the leather sample. Chromium and consequently Cr_2O_3 was determined in the prepared sample solutions by using inductively coupled plasma atomic emission spectrometry (ICP-AES) and flame atomic absorption spectrometry (AAS). The obtained results revealed that the direct acid digestion procedure by requiring minimum additive chemicals and no fusion step without leaving any residue represents a convenient procedure for the complete dissolution of leather samples that can be analyzed for Cr using an appropriate analytical technique such as AAS or ICP-AES. The accuracy of the conventional method could be increased by increasing the Na_2CO_3/ K_2CO_3/ borax mixture from 4-fold that of the leather sample to 5-fold and, in addition, by raising the ashing temperature from 800℃ to 900℃ in order to ensure the complete dissolution of the sample.
机译:将三种不同的样品制备程序应用于皮革样品,代表了鞣制过程的四个不同步骤,即在鞣制步骤(湿蓝)之后,复鞣步骤(结皮)之后,正常整理之后和硅整理过程之后。样品制备程序是常规程序,其中将样品在800℃下与Na_2CO_3,K_2CO_3和硼砂的混合物熔融,然后溶解在沸水中并过滤。其他两个建议的步骤是灰化/熔融步骤,其中将皮革样品在1000℃灰化,然后与NaOH,Na_2O_2和Na_2CO_3进行碱熔融步骤,而在第二个步骤中,将皮革样品与浓HNO_3回流。两种方法均导致皮革样品完全溶解。通过使用电感耦合等离子体原子发射光谱法(ICP-AES)和火焰原子吸收光谱法(AAS)测定了制备的样品溶液中的铬以及因此的Cr_2O_3。获得的结果表明,直接酸消解程序需要的添加剂化学物质最少,没有任何残留物的融合步骤,代表了皮革样品完全溶解的便捷程序,可以使用适当的分析技术(例如AAS或ICP)分析皮革中的Cr -AES。通过将Na_2CO_3 / K_2CO_3 /硼砂混合物的浓度从皮​​革样品的4倍提高到5倍,并且将灰化温度从800℃提高到900℃,可以提高传统方法的精度。确保样品完全溶解。

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