WO2020233150A1 - 一种食用盐中氯化钠含量的计算方法 - Google Patents

一种食用盐中氯化钠含量的计算方法 Download PDF

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WO2020233150A1
WO2020233150A1 PCT/CN2020/071695 CN2020071695W WO2020233150A1 WO 2020233150 A1 WO2020233150 A1 WO 2020233150A1 CN 2020071695 W CN2020071695 W CN 2020071695W WO 2020233150 A1 WO2020233150 A1 WO 2020233150A1
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sample
content
solution
silver nitrate
chloride ion
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PCT/CN2020/071695
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楼超群
周骏贵
张驰
胡飞杰
顾慧丹
余恒琳
申蓉
王晓丽
朱毛毛
郭楠歆
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南京市产品质量监督检验院
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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  • the invention relates to the technical field of a method for detecting sodium chloride content in edible salt.
  • the supervision and spot check of edible salt is an important means to supervise the quality and safety of edible salt after the reform of the salt industry.
  • the inspection items of edible salt include sodium chloride, lead, total arsenic, cadmium, total mercury, barium, potassium chloride, ferrous potassium chloride , Iodine and other parameters, the current inspection method is mainly based on the "National Food Safety Standard Determination of Salt Index" (GB 5009.42-2016), in which the determination of sodium chloride content needs to be calculated according to the method of calcium sulfate, magnesium sulfate, sodium sulfate, and chlorine. The content of calcium chloride, magnesium chloride and potassium chloride, the remaining chloride ion is calculated as sodium chloride (wet basis) content.
  • the calculation process is very cumbersome. It is necessary to calculate the sodium chloride content in seven steps, and finally calculate the sodium chloride (wet basis) based on the moisture content. ⁇ )Content. In the inspection and testing process, only the sodium chloride (dry basis) parameter is divided into eight steps, which causes the subsequent calculation to occupy a lot of time and energy, low efficiency, and the calculation process is extremely error-prone.
  • the purpose of the present invention is to provide a method for calculating the sodium chloride content in edible salt with simple calculation process, small data volume and accurate calculation results.
  • a method for calculating the content of sodium chloride in edible salt which is characterized by comprising the following steps:
  • the drying temperature is set to 140°C ⁇ 2°C, and the mass difference between the two before and after drying is less than 5mg, which is the constant weight;
  • step 1) After dissolving the sample in step 1), use potassium chromate as an indicator and titrate with silver nitrate standard titration solution to determine the chloride ion content.
  • the potassium chromate indicator of the present invention is as follows: weigh 10 g of potassium chromate and dissolve in 100 ml of water, add silver nitrate solution dropwise with stirring until a reddish brown precipitate appears, and filter.
  • Step 2) of the present invention specifically includes: weighing 25g of the pulverized sample into a 400ml beaker, adding 200ml of water, heating, and stirring with a glass rod until all is dissolved; after cooling, transfer to a 500ml volumetric flask, add water to a constant volume, and shake well ; Pipette 25ml of the sample solution in a 250ml volumetric flask, dilute to volume with water, and shake well; then determine to draw 25ml of the diluted sample solution into a 150ml Erlenmeyer flask, add water to 50ml, add 4 drops of potassium chromate indicator, while stirring Titrate with silver nitrate standard titration solution until a stable orange-red color appears in the suspension as the end point; at the same time do a blank test.
  • X 1 is the chloride ion content in the sample, expressed in %;
  • V 1 is the amount of silver nitrate standard titration solution in ml;
  • V 0 is the amount of silver nitrate standard titration solution in blank test, in ml;
  • C is nitric acid
  • concentration of silver standard titration solution, the unit is mol/l; 35.453 is the molar mass of chloride ion, the unit is g/mol; f is the dilution multiple of the sample solution;
  • m is the mass of the sample, the unit is g; 100 and 1000 are the units Conversion factor; the calculation result is expressed to two decimal places.
  • Edible salt is a substance that is completely soluble in water and exists in the form of ions in the water. The anion and cation must be balanced, otherwise it will be charged.
  • the present invention is based on the electrochemical equilibrium method as the basic principle, which is in line with reality, so it is simpler and more effective than ordinary calculation methods.
  • the present invention performs calculation directly after sampling the relevant data of the sample, which makes the operation more convenient and the calculation efficiency higher.
  • the present invention has a positive effect on driving the overall efficiency of the entire edible salt testing industry, and provides a solution for other similar parameter calculations.
  • a method for calculating sodium chloride content in edible salt includes the following steps:
  • the drying temperature is set to 140°C ⁇ 2°C, and the mass difference between the two before and after drying is less than 5mg, which is the constant weight;
  • step 1) After dissolving the sample in step 1), use potassium chromate as an indicator and titrate with silver nitrate standard titration solution to determine the chloride ion content.
  • the potassium chromate indicator of the present invention is as follows: weigh 10 g of potassium chromate and dissolve in 100 ml of water, add silver nitrate solution dropwise with stirring until red-brown precipitation appears, and filter.
  • Step 2) of the present invention specifically includes: weighing 25g of the pulverized sample into a 400ml beaker, adding 200ml of water, heating, and stirring with a glass rod until all is dissolved; after cooling, transfer to a 500ml volumetric flask, add water to a constant volume, and shake well ; Pipette 25ml of the sample solution in a 250ml volumetric flask, dilute to volume with water, and shake well; then determine to draw 25ml of the diluted sample solution into a 150ml Erlenmeyer flask, add water to 50ml, add 4 drops of potassium chromate indicator, while stirring Titrate with silver nitrate standard titration solution until a stable orange-red color appears in the suspension as the end point; at the same time do a blank test.
  • X 1 is the chloride ion content in the sample, expressed in %;
  • V 1 is the amount of silver nitrate standard titration solution in ml;
  • V 0 is the amount of silver nitrate standard titration solution in blank test, in ml;
  • C is nitric acid
  • concentration of silver standard titration solution, the unit is mol/l; 35.453 is the molar mass of chloride ion, the unit is g/mol; f is the dilution multiple of the sample solution;
  • m is the mass of the sample, the unit is g; 100 and 1000 are the units Conversion factor; the calculation result is expressed to two decimal places.
  • the above table is the calculated results of the sodium chloride content of the two batches of samples after calculation. You can compare the country's relevant standards for sodium chloride content in edible salt to determine whether the corresponding samples meet the standards.

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Abstract

一种食用盐中氯化钠含量的计算方法，包括如下步骤：1)水分测定：按照直接干燥法，将干燥温度设定为140℃±2℃，干燥至前后两次的质量差小于5㎎，即为恒重；2)氯离子测定：将步骤1)中的样品溶解后，用铬酸钾作为指示剂，用硝酸银标准滴定溶液滴定，测定氯离子的含量。该方法计算过程简单，数据量较小，计算结果准确。

Description

一种食用盐中氯化钠含量的计算方法 技术领域
本发明涉及食用盐中氯化钠含量检测方法的技术领域。
背景技术
食用盐的监督抽查工作是盐业改革后监督食用盐质量安全的重要手段，食用盐检验项目包括氯化钠、铅、总砷、镉、总汞、钡、氯化钾、亚铁氯化钾、碘等参数，目前的检验方法主要依据《食品安全国家标准食盐指标的测定》(GB 5009.42-2016)，其中氯化钠含量的测定需根据方法依次计算硫酸钙、硫酸镁、硫酸钠、氯化钙、氯化镁、氯化钾的含量，剩余氯离子计算为氯化钠(湿基)含量，计算过程非常繁琐，需分七步测算氯化钠含量，最后根据水分含量计算氯化钠(湿基)含量。在检验检测过程中，仅氯化钠(干基计)参数一项就分为八个步骤，导致后续计算占据大量的时间及精力，效率低下，且计算过程极易出错。
发明内容
本发明目的是提供一种计算过程简单，数据量较小，计算结果准确的食用盐中氯化钠含量的计算方法。
一种食用盐中氯化钠含量的计算方法，其特征在于包括如下步骤：
1)水分测定：
按照直接干燥法，将干燥温度设定为140℃±2℃，干燥至前后两次的质量差小于5㎎，即为恒重；
2)氯离子测定：
将步骤1)中的样品溶解后，用铬酸钾作为指示剂，用硝酸银标准滴定溶液滴定，测定氯离子的含量。
比较好的是，本发明的铬酸钾指示剂为：称取10g铬酸钾溶于100ml水中，搅拌下滴加硝酸银溶液至出现红棕色沉淀，过滤。
本发明的步骤2)具体包括：称取25g粉碎后的样品于400ml烧杯中，加入200ml的水，加热，用玻璃棒搅拌至全部溶解；冷却后转移至500ml容量瓶，加水定容，摇匀；吸取25ml试样溶液于250ml容量瓶中，用水定容，摇匀；然后测定吸取25ml稀释的试样溶液于150ml锥形瓶中，加水至50ml，加入4滴铬酸钾指示剂，边搅拌边用硝酸银标准滴定溶液滴定，直至悬浊液中出现稳定的桔红色为终点；同时做空白试验。
试样中氯离子含量按照公式(1)进行结算：
Figure PCTCN2020071695-appb-000001
其中X 1是试样中氯离子含量，用％表示；V 1是硝酸银标准滴定溶液的用量，单位为ml；V 0是空白试验硝酸银标准滴定溶液的用量，单位为ml；C是硝酸银标准滴定溶液的浓度，单位为mol/l；35.453是氯离子的摩尔质量，单位为g/mol；f是试样液稀释倍数；m是试样质量，单 位为g；100、1000是单位转换系数；计算结果表示到小数点后两位。
本发明采样上述技术方案，与现有技术相比具有如下优点：
1、食用盐是全溶于水的物质，且以离子的形式存在水中，必然是阴阳离子保持平衡，否则会带电。本发明基于电化学平衡法作为基础原理是符合实际的，因此比起普通的计算方法更加简单和有效。
2、本发明根据对样品的相关数据进行采样后，直接进行计算，操作更加方便，计算效率更高。
3、本发明对带动整个食用盐检测行业的整体效能有积极的推动作用，并对其他类似的参数计算提供了可借鉴的解决方案。
具体实施方式
一种食用盐中氯化钠含量的计算方法，包括如下步骤：
1)水分测定：
按照直接干燥法，将干燥温度设定为140℃±2℃，干燥至前后两次的质量差小于5㎎，即为恒重；
2)氯离子测定：
将步骤1)中的样品溶解后，用铬酸钾作为指示剂，用硝酸银标准滴定溶液滴定，测定氯离子的含量。
本发明的铬酸钾指示剂为：称取10g铬酸钾溶于100ml水中，搅拌下滴加硝酸银溶液至出现红棕色沉淀，过滤。
本发明的步骤2)具体包括：称取25g粉碎后的样品于400ml烧杯中，加入200ml的水，加热，用玻璃棒搅拌至全部溶解；冷却后转移至500ml容量瓶，加水定容，摇匀；吸取25ml试样溶液于250ml容量瓶中，用水定容，摇匀；然后测定吸取25ml稀释的试样溶液于150ml锥形瓶中，加水至50ml，加入4滴铬酸钾指示剂，边搅拌边用硝酸银标准滴定溶液滴定，直至悬浊液中出现稳定的桔红色为终点；同时做空白试验。
试样中氯离子含量按照公式(1)进行结算：
Figure PCTCN2020071695-appb-000002
其中X 1是试样中氯离子含量，用％表示；V 1是硝酸银标准滴定溶液的用量，单位为ml；V 0是空白试验硝酸银标准滴定溶液的用量，单位为ml；C是硝酸银标准滴定溶液的浓度，单位为mol/l；35.453是氯离子的摩尔质量，单位为g/mol；f是试样液稀释倍数；m是试样质量，单位为g；100、1000是单位转换系数；计算结果表示到小数点后两位。
基于电化学原理的食用盐中氯化钠含量的计算方法
Figure PCTCN2020071695-appb-000003
上表中是经过计算后得到的两批样品的氯化钠含量的计算结果，可对照国家对于食用盐中氯化钠含量的相关标准，确定对应的样品是否符合标准。

Claims (4)

  1. 一种食用盐中氯化钠含量的计算方法，其特征在于包括如下步骤：
    1)水分测定：
    按照直接干燥法，将干燥温度设定为140℃±2℃，干燥至前后两次的质量差小于5㎎，即为恒重；
    2)氯离子测定：
    将步骤1)中的样品溶解后，用铬酸钾作为指示剂，用硝酸银标准滴定溶液滴定，测定氯离子的含量。
  2. 根据权利要求1所述的食用盐中氯化钠含量的计算方法，其特征在于上述铬酸钾指示剂为：称取10g铬酸钾溶于100ml水中，搅拌下滴加硝酸银溶液至出现红棕色沉淀，过滤。
  3. 根据权利要求1或2所述的食用盐中氯化钠含量的计算方法，其特征在于上述步骤2)具体包括：称取25g粉碎后的样品于400ml烧杯中，加入200ml的水，加热，用玻璃棒搅拌至全部溶解；冷却后转移至500ml容量瓶，加水定容，摇匀；吸取25ml试样溶液于250ml容量瓶中，用水定容，摇匀；然后测定吸取25ml稀释的试样溶液于150ml锥形瓶中，加水至50ml，加入4滴铬酸钾指示剂，边搅拌边用硝酸银标准滴定溶液滴定，直至悬浊液中出现稳定的桔红色为终点；同时做空白试验。
  4. 试样中氯离子含量按照公式(1)进行结算：
    Figure PCTCN2020071695-appb-100001
    其中X 1是试样中氯离子含量，用％表示；V 1是硝酸银标准滴定溶液的用量，单位为ml；V 0是空白试验硝酸银标准滴定溶液的用量，单位为ml；c是硝酸银标准滴定溶液的浓度，单位为mol/l；35.453是氯离子的摩尔质量，单位为g/mol；f是试样液稀释倍数；m是试样质量，单位为g；100、1000是单位转换系数；计算结果表示到小数点后两位。
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CN113607665A (zh) * 2021-07-23 2021-11-05 华能国际电力股份有限公司济宁电厂 一种氨水中杂质氯化物的检测方法
CN113970500A (zh) * 2021-10-27 2022-01-25 北京新风航天装备有限公司 一种油污固废含油率快速测定方法
CN113970500B (zh) * 2021-10-27 2023-08-29 北京新风航天装备有限公司 一种油污固废含油率快速测定方法
CN115420696A (zh) * 2022-09-19 2022-12-02 安徽超威环保科技有限公司 一种四元水盐体系组分含量的检测方法

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