阅读说明：本技术 一种定量检测固态危废氯离子的方法 (Method for quantitatively detecting solid hazardous waste chloride ions ) 是由 李海军 鲁凤春 李保军 王巍 王�华 于 2020-06-19 设计创作，主要内容包括：本发明公开了一种定量检测固态危废氯离子的方法,具体涉及氯离子检测技术领域,具体步骤如下：步骤一：首先,建立一条熟料标准曲线,其中,熟料标准曲线制作方法如下；1)采用波长色散型X射线荧光光谱仪,建立一条熟料标准曲线,增加热生料标准样品2个,2)为降低熟料的颗粒度效应对分析结果造成的偏差,采用振动磨对样品进行粉末1-5分钟,加入硬脂酸作为助磨剂。本发明结果准确,常规荧光分析不能准确测量危废的数值,现在的方法由于主要基体都是同一个熟料,克服了荧光分析中的矿物效应和颗粒度效应,危废中带人的氯离子由于加入大量熟料被稀释,浓度范围大幅缩短,且有数据支撑。(The invention discloses a method for quantitatively detecting solid hazardous waste chloride ions, and particularly relates to the technical field of chloride ion detection, wherein the method comprises the following specific steps: the method comprises the following steps: firstly, establishing a clinker standard curve, wherein the clinker standard curve is manufactured by the following method; 1) establishing a clinker standard curve by adopting a wavelength dispersion type X-ray fluorescence spectrometer, adding 2 hot raw material standard samples, 2) in order to reduce the deviation of the granularity effect of the clinker on the analysis result, performing powder grinding on the samples for 1-5 minutes by adopting a vibration mill, and adding stearic acid as a grinding aid. The method has accurate result, the conventional fluorescence analysis can not accurately measure the numerical value of the dangerous waste, the existing method overcomes the mineral effect and the granularity effect in the fluorescence analysis because the main matrixes are the same clinker, and the concentration range is greatly shortened because the manned chloride ions in the dangerous waste are diluted by adding a large amount of clinker, and the dangerous waste is supported by data.)

1. A method for quantitatively detecting solid hazardous waste chloride ions is characterized by comprising the following steps: the method comprises the following specific steps:

the method comprises the following steps: firstly, establishing a clinker standard curve, wherein the clinker standard curve is manufactured by the following method:

1) establishing a clinker standard curve by adopting a wavelength dispersion type X-ray fluorescence spectrometer, and adding 2 standard samples of hot raw materials;

2) performing powder grinding on a sample for 1-5 minutes by adopting a vibration mill, and adding stearic acid as a grinding aid;

3) taking the ground sample for tabletting;

4) measuring two standard samples by using an original clinker program, and performing curve regression correction;

step two: the detection method for the unknown sample comprises the following specific steps:

1) taking 1kg of clinker aggregate in the conventional production, grinding and mixing uniformly, and storing as a sample 1;

2) weighing 30g of clinker sample and 0.2g of stearic acid, grinding for 1min by using a vibration mill, tabletting, and quantitatively detecting the clinker by using a newly-built curve, wherein the numerical value is used as original data;

3) taking about 20g of solid hazardous waste sample, drying at about 100-120 ℃ for 0.5-2 hours, calculating the water content in the sample, and storing as sample 2;

4) accurately weighing 30g of clinker sample to 1%, accurately weighing 1 +/-0.5 g of dried hazardous waste sample and 0.2g of stearic acid, grinding for 1min by using a vibration mill, tabletting and storing as a sample 3;

5) measuring the composition of the mixed sample;

X＝{[C*(α+β+γ)-α*ω/β]}*(1-)

wherein C is the measured value of the chloride ion content of the sample 3;

α is sample 1 weight;

β is sample 2 weight;

gamma is stearic acid weight;

omega is the measured value of the chloride ion content of the sample 1

Sample 2 moisture content.

2. The method for quantitatively detecting the solid-state dangerous waste chloride ions according to claim 1, characterized in that: in the second step, the diameter of clinker grinding is set to be 70-120 um.

3. The method for quantitatively detecting the solid-state dangerous waste chloride ions according to claim 1, characterized in that: clinker is clinker obtained by grinding cement raw materials into raw materials and then calcining the raw materials.

4. The method for quantitatively detecting the solid-state dangerous waste chloride ions according to claim 1, characterized in that: in the first step, the ratio of stearic acid to the sample is 0.2:30.

Technical Field

The invention relates to the technical field of chloride ion detection, in particular to a method for quantitatively detecting solid-state dangerous waste chloride ions.

Background

Cement: a powdered hydraulic inorganic cementitious material. After water is added and stirred, the mortar can be hardened in the air or in water and can firmly bond sand, stone and other materials together, the early mixture of lime and volcanic ash is very similar to the modern lime-volcanic ash cement, and concrete made of broken stone cemented by the mortar not only has higher strength, but also can resist the erosion of fresh water or salt-containing water after being hardened. It has long been used as an important cementing material and is widely applied to engineering of civil construction, water conservancy, national defense and the like.

The chloride ion is one of the important indexes of the cement quality, the national standard 175 requires that the content of the chloride ion in the cement cannot exceed 0.006 percent, the content of a plurality of dangerous waste chloride ions is very high, the content of the dangerous waste chloride ions is accurately detected, and the method has very important significance for controlling the cement quality. However, because the chloride ion compounds in the hazardous waste fluctuate greatly, the conventional (or current commonly used) detection method (mainly fluorescence semi-quantitative analysis) cannot meet the analysis requirements, because semi-quantitative software is a qualitative analysis program, the relative analysis error is large, and because the analysis result needs to be converted into the loss on ignition, but because the chemical combination form of the chloride elements in the hazardous waste is different, the volatile amount after 950 ℃ ignition is unstable, and the volatile amount is high or low, the result cannot be judged.

Disclosure of Invention

In order to overcome the above defects in the prior art, embodiments of the present invention provide a method for quantitatively detecting solid-state hazardous waste chloride ions, which has accurate results, and the conventional fluorescence analysis cannot accurately measure the numerical value of the hazardous waste.

In order to achieve the purpose, the invention provides the following technical scheme: a method for quantitatively detecting solid hazardous waste chloride ions comprises the following specific steps:

the method comprises the following steps: firstly, establishing a clinker standard curve, wherein the clinker standard curve is manufactured by the following method:

1) establishing a clinker standard curve by adopting a wavelength dispersion type X-ray fluorescence spectrometer, and adding 2 standard samples of hot raw materials;

2) in order to reduce the deviation of the granularity effect of the clinker on the analysis result, performing powder grinding on a sample for 1-5 minutes by adopting a vibration mill, and adding stearic acid as a grinding aid;

3) taking the ground sample for tabletting;

4) two standard samples were measured using the raw clinker procedure and corrected for curve regression.

Step two: the detection method for the unknown sample comprises the following specific steps:

1) taking 1kg of clinker aggregate in the conventional production, grinding and mixing uniformly, and storing as a sample 1;

2) weighing 30g of clinker sample and 0.2g of stearic acid, grinding for 1min by using a vibration mill, tabletting, and quantitatively detecting the clinker by using a newly-built curve, wherein the numerical value is used as original data;

3) taking about 20g of solid hazardous waste sample, drying at about 100-120 ℃ for 0.5-2 hours, calculating the water content in the sample, and storing as sample 2;

4) accurately weighing 30g of clinker sample to 1%, accurately weighing 1 +/-0.5 g of dried hazardous waste sample and 0.2g of stearic acid, grinding for 1min by using a vibration mill, tabletting and storing as a sample 3;

5) measurement of the composition of the mixed sample:

X＝{[C*(α+β+γ)-α*ω/β]}*(1-)

wherein C is the measured value of the chloride ion content of the sample 3;

α is sample 1 weight;

β is sample 2 weight;

gamma is stearic acid weight;

omega is the measured value of the chloride ion content of the sample 1

Sample 2 moisture content.

In a preferred embodiment, in step two, the clinker grinding diameter is set at 70-120 um.

In a preferred embodiment, in step one, the ratio of stearic acid to sample is 0.2:30.

In a preferred embodiment, the wavelength-dispersive X-ray fluorescence spectrometer is an apparatus for analyzing a material composition by exciting atoms in a material to be measured with primary X-rays or other photon sources to generate fluorescence (secondary X-rays), and is also called an XRF spectrometer, both dispersive and non-dispersive, and an apparatus for analyzing a material composition by exciting atoms in a material to be measured with X-rays or other photon sources to generate fluorescence (secondary X-rays), both dispersive and non-dispersive, and dispersive is classified into wavelength-dispersive and energy-dispersive types.

In a preferred embodiment, clinker refers to clinker obtained by grinding cement raw materials into raw meal and then calcining the raw meal.

The invention has the technical effects and advantages that:

1. the method is simple and easy to operate, the speed is high, the measurement time of one sample can be controlled within 2min, and the detection efficiency is improved;

2. the existing method overcomes mineral effect and granularity effect in fluorescence analysis because main matrixes are the same clinker, and concentration range is greatly shortened because a large amount of clinker is added to dilute chloride ions with people in hazardous waste (the former range may be 0-80, the range can be controlled to be 0-5 according to actual conditions after mixing, and only the amount of the hazardous waste needs to be reduced), and the method is supported by data.

3. Harm to personnel reduces because the mode that contacts useless volume of danger in the past to personnel has changed, leads to the useless volume of personnel contact danger to reduce.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.