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Method for simultaneously detecting boric acid and borax
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A technology of borax and boric acid, applied in the field of chemical analysis, which can solve problems such as indistinguishability and errors
Active Publication Date: 2015-05-13
谱尼测试集团深圳有限公司
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These methods cannot distinguish between samples containing borax or boric acid
[0008] The sample is directly subjected to acid digestion or microwave digestion. Since some compounded boron will also be dissolved (such as boron in borosilicate), boron is determined as borax and boric acid, and the measurement results are often far more than SVHC 0.1% limit, causing a large error
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Embodiment 1
[0022] Analysis steps:
[0023] Take boron phenolic resin fine particles, pulverize them with a high-speed pulverizer, and pass through an 80-mesh sieve to obtain a powder sample. Take 0.4347g sample into a polytetrafluoroethylene beaker, add 30mL of secondary water and 1mL of phosphoric acid, extract by boiling for 20min on the electric heating plate, remove and cool, filter with qualitative filter paper, wash the filter paper 3 times with 5mL of secondary water respectively. Add 10mL of mixed acid of nitric acid and perchloric acid (10+1) to the obtained filtrate, digest on a hot plate, heat and digest until white smoke is emitted, remove and cool, then add 2mL of water, continue heating to drive out acid, until residual in the beaker When about 1mL of liquid, remove and cool to room temperature. Transfer to a 100mL plastic volumetric flask with water, and make up to the mark with water. The total boron B1 content in the sample determined by ICP-AES was 2.19×10 3 mg / kg. ...
Embodiment 2
[0026] Analysis steps: take glass fiber reinforced polyester resin masterbatch, crush the sample through 80 mesh sieve, take 5.0214g powder sample in a 100mL porcelain crucible, first carbonize it on an electric furnace until it does not emit smoke, and then put it in a muffler at 550°C High-temperature ashing in the furnace for 4 hours, the ash content was 47.2%. Take 0.3228g of ash into a polytetrafluoroethylene beaker, add 20mL of secondary water and 1mL of phosphoric acid, extract by boiling on a hot plate for 20min, after cooling, filter with qualitative filter paper, wash the filter paper 3 times with 5mL of secondary water respectively. Add 10mL of mixed acid of nitric acid and perchloric acid (10+1) to the filtrate, digest on a hot plate, heat and digest until white smoke is emitted, remove and cool, then add about 2mL of water, continue to heat to catch the acid until it reaches the beaker When about 1mL of liquid remains, remove and cool to room temperature. Transfe...
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Abstract
The invention discloses a method for simultaneously detecting substances of very high concern (SVHC) boric acid and borax of registration, evaluation, authorization and restriction of chemicals (REACH) law of European Union, and belongs to the fields of analysis and detection. The method comprises the following steps: cutting, crushing and sieving a sample; directly taking the sample powder or ash obtained after the sample powder is ashed at high temperature, adding water and a small amount of phosphoric acid and performing micro-boiling extraction, filtering by using filtering paper, digesting the filtrate with acid, and measuring the total boron (B1) content by an inductive coupling plasma atomic emission spectrum; and taking part of ash, adding ethanol, performing vibrating extraction, filtering by using filtering paper, discarding the filtrate, volatilizing ethanol from the sample on the residual filtering paper at room temperature, transferring to a beaker, adding water and a small amount of phosphoric acid and performing micro-boiling extraction, filtering by using filtering paper, digesting the filtrate with acid, and measuring the total boron (B2) content by an inductive coupling plasma atomic emission spectrum, wherein the B2 content is the boron content of the borax, the difference obtained by subtracting B2 from B1 is the boron content of the boric acid, and the boric acid content and the borax content of the sample can be known through conversion. The method is suitable for simultaneously detecting the content of SVHC boric acid and borax of the REACH law of European Union, simple, quick, high in accuracy and low in interference.
Description
【Technical field】 [0001] The invention belongs to the field of chemical analysis, in particular to a method for simultaneous detection of boric acid and borax. 【Background technique】 [0002] Since June 2007, the European Union's regulations on the preventive management of all chemicals entering its market "Registration, Evaluation, Authorization and Restriction of Chemicals, Chemical Registration, Evaluation, Authorization and Restriction", referred to as REACH. And regularly publish the list of substances of very high concern (Substances of very high chemicals, referred to as SVHC). Generally speaking, the content of chemical substances in the SVHC list is greater than or equal to 0.1% in articles, or the total content of chemical substances in them exceeds 1 ton per year. , substance classification, use of the substance in the article and the use of the article, the tonnage range of the substance, etc. to report to the European Chemicals Administration (ECHA). [0003] ...
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