A method for determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics

Abstract

The invention relates to a method for determining the content of perylene cyanol 29 in paint, textile and plastic, comprising the following steps: 1) sample pretreatment: cutting a textile sample into pieces, or crushing a plastic sample, wherein the size of the sample does not exceed 0.5*0.5*0.5 mm, mixing the crushed textile samples or plastic samples uniformly, putting them into a clean and dry ziplock bag, sealing and storing them for standby use; or mixing the paint sample uniformly for standby use; 2) sample extraction: weighing an appropriate amount of sample, adding DMSO and NaOH solution for shaking extraction, transferring the sample to a sample bottle after derivatization, and waiting for testing; 3) using HPLC-DAD to determine the concentration of perylene cyanol 29 derivatives in the sample extraction solution; 4) calculating the content of perylene cyanol 29 in the sample according to the concentration of perylene cyanol 29 derivatives in the sample extraction solution; the determination method provided by the invention is fast and simple, and can realize the accurate determination of the content of perylene cyanol 29 in paint, textile and plastic.

Description

[Technical field]

[0001] The invention belongs to the technical field of analytical chemistry, in particular to a method for determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics. [Background Technology]

[0002] Pigment Violet 29 is an organic functional dye. Due to its good chemical, thermal and light stability, wide absorption spectrum and high fluorescence quantum yield, it plays a role in the traditional dye industry and is also widely used in related fields such as organic photoconductive materials, organic electroluminescent materials, laser dyes, and chemiluminescent pigments. Pigment Violet 29 is red to jujube red in color and has excellent light and weather fastness. It is mainly used in metal decorative paints. Its high thermal stability makes it suitable for coloring plastics processed at high temperatures, and can also be used for coloring polyester fiber spinning.

[0003] At present, there is no detection method for the content of Perylene Brilliant Purple 29 at home and abroad. Perylene Brilliant Purple 29 compound is insoluble in water and almost insoluble in most organic solvents such as toluene and acetone. Although it is soluble in concentrated sulfuric acid, concentrated sulfuric acid is highly corrosive and oxidizing, and the safety risk of daily operation is high. Obviously, conventional detection methods are not suitable for the detection of Perylene Brilliant Purple 29. Therefore, it is urgent to establish a detection method for the content of Perylene Brilliant Purple 29 in paints, textiles and plastics. [Summary of the invention]

[0004] The purpose of the present invention is to solve the above-mentioned shortcomings and provide a method for determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics. The content of Perylene Brilliant Purple 29 is determined by extraction under alkaline conditions and derivatization, and then liquid chromatography-ultraviolet spectrometer (hereinafter referred to as HPLC-DAD) is used to determine the content of Perylene Brilliant Purple 29. The determination method is fast and simple, and can achieve accurate determination of the content of Perylene Brilliant Purple 29 in paints, textiles and plastics.

[0005] To achieve the above purpose, a method for determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics is designed, comprising the following steps:

[0006] 1) Sample pretreatment: Cut the textile samples into pieces with scissors, or crush the plastic samples with a crusher, so that the sample size does not exceed 0.5mm*0.5mm*0.5mm. Mix the crushed textile samples or plastic samples evenly, put them into a clean and dry ziplock bag, seal and store them for later use; or mix the paint samples evenly and set them aside;

[0007] 2) Sample extraction: Weigh an appropriate amount of sample, add DMSO and NaOH solution to shake and extract, transfer to a sample bottle after derivatization, and wait for testing;

[0008] 3) using HPLC-DAD to determine the concentration of the perylene brilliant purple 29 derivative in the sample extraction solution;

[0009] 4) According to the concentration of the perylene brilliant purple 29 derivative in the sample extraction solution obtained in step 3), the content of perylene brilliant purple 29 in the sample is calculated.

[0010] Further, in step 2), weigh 0.1 g of sample, add 10 mL of DMSO and 50 uL of 5% NaOH solution, shake at 300 rpm for 6 hours; add 1 mL of ethyl bromide and 5 mL of toluene; seal and place in a 95 degree Celsius oven for 95 minutes; then cool to room temperature, add 10 mL of water, shake at 300 rpm for 2 minutes, centrifuge at 9500 rpm for 2 minutes, filter the toluene layer into a sample bottle for testing.

[0011] Furthermore, in step 2), the reaction formula for generating the perylene brilliant purple 29 derivative is:

[0012]

[0013] Furthermore, the steps for preparing the standard solution of Perylene Brilliant Purple Red 29 are as follows:

[0014] (1) Weigh 5 mg of Perylene Brilliant Purple 29 standard, add 100 mL of DMSO and mix well to prepare a 50 mg / L Perylene Brilliant Purple 29 standard stock solution;

[0015] (2) Measure 10 mL of the stock solution into a 100 mL volumetric flask and dilute to the mark with DMSO. The concentration is now 5 mg / L.

[0016] (3) taking 10 mL of the 5 mg / L standard solution and derivatizing it according to the process in step 2) to prepare 10 mg / L perylene brilliant purple red 29;

[0017] (4) Dilute 10 mg / L Perylene Brilliant Purple 29 with toluene to prepare a standard curve of 0.2, 0.5, 1, 2, 5, and 10 for analysis.

[0018] Further, in step 3), the determination conditions of the HPLC-DAD are:

[0019] .

[0020] Furthermore, in step 4), the concentration of the perylene brilliant purple 29 derivative in the extraction solution is converted to the content of perylene brilliant purple 29 in the sample, and the external standard method is used for quantification according to the solvent calibration curve, and the minimum quantitative concentration is 10 mg / kg.

[0021] Further, in step 4), the calculation formula of Perylene Brilliant Purple 29 is,

[0022] in,

[0023] C: The concentration of sample B in mg / L obtained from the standard curve;

[0024] V: final fixed volume mL;

[0025] m: sample mass g;

[0026] DF: dilution factor.

[0027] Furthermore, step 4) also includes qualitative and quantitative steps:

[0028] (1) Qualitative analysis: By comparing the retention time of the sample peak with that of the standard peak, and comparing the full scan spectrum of the sample peak with that of the standard substance, it is determined whether Perylene Brilliant Purple Red 29 is detected in the sample;

[0029] (2) Quantification: Quantification was performed using the external standard method using a calibration curve.

[0030] Compared with the prior art, the present invention has the following advantages:

[0031] (1) The present invention is a method for directly determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics by HPLC-DAD after extraction with an organic solvent and an alkaline solution and derivatization;

[0032] (2) The present invention is not only fast and simple to measure, but also can accurately measure the content of Perylene Brilliant Purple Red 29 in paints, textiles and plastics, with a minimum quantitative concentration of 10 mg / kg;

[0033] (3) The present invention solves the problem of the method for measuring the content of Perylene Brilliant Purple 29 in paints, textiles and plastics, and fully meets the requirements for monitoring the content of Perylene Brilliant Purple 29 in paints, textiles and plastics. [Drawings]

[0034] Figure 1 is a chromatogram of the perylene brilliant purple 29 derivative of the present invention;

[0035] Figure 2 It is the spectrum of the perylene brilliant purple 29 derivative of the present invention;

[0036] Figure 3 It is a schematic diagram of the mechanism of generating the perylene brilliant purple 29 derivative in the reaction system of the present invention. [Specific implementation method]

[0037] The invention belongs to the technical field of analytical chemistry. Aiming at the problem that although Perylene Brilliant Purple 29 is added but there is no method for detecting the content thereof, a method is provided in which the content of Perylene Brilliant Purple 29 in paints, textiles and plastics is determined by HPLC-DAD after extraction under alkaline conditions and the derivatives are derivatized.

[0038] The main principle of the present invention is: extracting the perylene brilliant purple 29 in the sample with an organic solution and a sodium hydroxide solution, derivatizing and filtering, and then using HPLC-DAD to determine the content of perylene brilliant purple 29 in the sample. The determination steps are as follows:

[0039] 1) Sample pretreatment: Cut the textile samples into pieces with scissors, or crush the plastic samples with a crusher, so that the sample size does not exceed 0.5mm*0.5mm*0.5mm; mix the crushed samples evenly, put them into a clean and dry ziplock bag, seal and store them for later use; or mix the paint samples evenly and set them aside;

[0040] 2) Sample extraction: Weigh 0.1 g sample, add 10 mL DMSO and 50 uL 5% NaOH solution; shake at 300 rpm for 6 hours; add 1 mL ethyl bromide and 5 mL toluene; seal and place in a 95 degree Celsius oven for 95 minutes; then cool to room temperature, add 10 mL water, shake at 300 rpm for 2 minutes; centrifuge at 9500 rpm for 2 minutes; filter the toluene layer into a sample bottle and analyze by HPLC-DAD;

[0041] In the above reaction system, the mechanism of generating the perylene brilliant purple 29 derivative is as shown in the attached Figure 3 shown.

[0042] The steps for preparing the standard solution of Perylene Brilliant Purple 29 are as follows:

[0043] (1) Weigh 5 mg of Perylene Brilliant Purple 29 standard, add 100 mL of DMSO and mix well to prepare a 50 mg / L Perylene Brilliant Purple 29 standard stock solution;

[0044] (2) Measure 10 mL of the stock solution into a 100 mL volumetric flask and dilute to the mark with DMSO. The concentration is now 5 mg / L.

[0045] (3) taking 10 mL of the 5 mg / L standard solution and derivatizing it according to the process in step 2) above to prepare 10 mg / L Perylene Brilliant Purple Red 29;

[0046] (4) Dilute 10 mg / L Perylene Brilliant Purple 29 with toluene to prepare a standard curve of 0.2, 0.5, 1, 2, 5, and 10 for analysis.

[0047] 3) Using HPLC-DAD to determine the concentration of the perylene brilliant purple 29 derivative in the sample extraction solution obtained in step 2), the determination conditions of the liquid chromatography-ultraviolet detector are:

[0048]

[0049]

[0050] 4) Calculate the content of Perylene Brilliant Purple 29 derivatives in the sample according to the concentration of Perylene Brilliant Purple 29 derivatives in the sample extraction solution obtained in step 3); specifically, the content of Perylene Brilliant Purple 29 in the sample is obtained by converting the concentration of Perylene Brilliant Purple 29 derivatives in the extraction solution, and quantify it by external standard method according to the solvent calibration curve, and the minimum quantitative concentration is 10 mg / kg.

[0051] The formula for calculating the purity of Perylene Brilliant Purple 29 is as follows:

[0052]

[0053] in,

[0054] C: Concentration of sample B obtained from the standard curve (mg / L)

[0055] V: final fixed volume (mL);

[0056] m: sample mass (g);

[0057] DF: dilution factor.

[0058] The present invention is further described below in conjunction with specific embodiments:

[0059] Example 1: Determination of the content of Perylene Brilliant Purple 29 in plastics

[0060] 1. Preparation of sample solution:

[0061] Crush the plastic with a crusher, and the size of the sample must not exceed 0.5mm*0.5mm*0.5mm; mix the crushed sample, put it into a clean and dry ziplock bag, seal it for storage and set aside; weigh 0.1g sample, add 10mL DMSO and 50uL 5% NaOH solution; shake it at 300rpm for 6 hours; add 1mL ethyl bromide and 5mL toluene; seal it and put it in a 95 degrees Celsius oven for 95 minutes; then cool it to room temperature, add 10mL water, shake it at 300rpm for 2min; centrifuge it at 9500rpm for 2min; filter the toluene layer into a sample bottle, and analyze it by HPLC-DAD.

[0062] 2. Set instrument parameters:

[0063]

[0064] 3. Qualitative and quantitative

[0065] 1) Qualitative analysis: By comparing the retention time of the sample peak with that of the standard peak, and comparing the full scan spectrum of the sample peak with that of the standard substance, it is determined whether Perylene Brilliant Purple 29 is detected in the sample.

[0066] 2) Quantification: Quantification was performed using the external standard method using a calibration curve.

[0067] 4. Calculation

[0068] According to the concentration of the derivative of Perylene Brilliant Purple 29 in the sample extraction solution, the content of Perylene Brilliant Purple 29 in the sample was calculated. After testing, the plastic contained 697 mg / kg Perylene Brilliant Purple 29.

[0069] In summary, the present invention is a method for determining the sample by liquid chromatography-ultraviolet detector after extraction and derivatization with DMSO NaOH solution. The determination method can accurately determine the content of perylene brilliant purple red 29 in paints, textiles and plastics, and the minimum quantitative concentration is 10 mg / kg.

[0070] The present invention is not limited to the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention shall be equivalent replacement methods and shall be included in the protection scope of the present invention.

Claims

1. A method for determining the content of Perylene Brilliant Purple 29 in paints, textiles and plastics, characterized in that: The following steps are involved: 1) Sample pretreatment: Cut the textile samples into pieces with scissors, or crush the plastic samples with a crusher, so that the sample size does not exceed 0.5mm*0.5mm*0.5mm. Mix the crushed textile samples or plastic samples evenly, put them into a clean and dry ziplock bag, seal and store them for later use; or mix the paint samples evenly and set them aside; 2) Sample extraction: Weigh an appropriate amount of sample, add DMSO and NaOH solution to shake and extract, transfer to a sample bottle after derivatization, and wait for testing; 3) using HPLC-DAD to determine the concentration of the perylene brilliant purple 29 derivative in the sample extraction solution; 4) calculating the content of Perylene Brilliant Purple 29 in the sample according to the concentration of the Perylene Brilliant Purple 29 derivative in the sample extraction solution obtained in step 3); In step 2), 0.1 g of sample was weighed, 10 mL of DMSO and 50 uL of 5% NaOH solution were added, and the mixture was shaken at 300 rpm for 6 hours; 1 mL of ethyl bromide and 5 mL of toluene were added; the mixture was sealed and placed in a 95°C oven for 95 minutes; the mixture was then cooled to room temperature, 10 mL of water was added, the mixture was shaken at 300 rpm for 2 minutes, and the mixture was centrifuged at 9500 rpm for 2 minutes, and the toluene layer was filtered into a sample bottle for testing; In step 2), the reaction formula for generating the perylene brilliant purple 29 derivative is: Wherein, R-Br is ethyl bromide; In step 3), the determination conditions of the HPLC-DAD are:

2. The method according to claim 1, characterized in that: In step 4), the concentration of the perylene brilliant purple 29 derivative in the extraction solution is converted into the content of perylene brilliant purple 29 in the sample, and the external standard method is used for quantification according to the solvent calibration curve, and the minimum quantitative concentration is 10 mg / kg.

3. The method according to claim 1, characterized in that Step 4) also includes qualitative and quantitative steps: (1) Qualitative analysis: By comparing the retention time of the sample peak with that of the standard peak, and comparing the full scan spectrum of the sample peak with that of the standard substance, it is determined whether Perylene Brilliant Purple Red 29 is detected in the sample; (2) Quantification: Quantification was performed using the external standard method based on the solvent calibration curve.

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