CN106769933A - 一种土壤中有效硅测定的改进方法 - Google Patents
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Classifications
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
Abstract
本发明公开了一种改进土壤有效硅含量的测定方法,属于环境保护领域。本发明是采用硅钼蓝分光光度法,在一定酸度下,硅与钼酸铵生成硅钼黄络合物,再将酸度提高,用抗坏血酸将硅钼黄络合物还原为硅钼蓝,进行比色。本法对土壤有效硅检出限为1.2mg/kg,相对标准偏差小于3.0%。本发明用盐酸替代硫酸调节pH,用2g/L抗坏血酸替代15g/L抗坏血酸来还原硅钼酸,比色波长由原来700nm调整为680nm,更大地提供了检测灵敏度和准确性。
Description
技术领域
本发明涉及境土壤检测技术领域,具体是涉及一种土壤中有效硅测定的改进方法。
背景技术
自然界中,硅的分布极广,仅次于氧,主要以二氧化硅和硅酸盐的形式存在,是农作物生长所需的重要营养元素之一,被国际土壤学届确认为继氮、磷、钾之后的第四种生长元素。因此研究土壤中硅非常必要。
农业部于2006年颁布了土壤有效硅的测定方法《土壤检测第15部分:土壤有效硅的测定》(NY/T 1121.15-2006),该法使用硫酸调节反应前溶液pH,用15g/L抗坏血酸将硅钼酸还原为硅钼蓝,在波长700nm处比色,通过测定蓝色深浅来测定硅浓度,但在实际实验中,发现该法反应显色不明显,测量灵敏度不高,本研究用盐酸替代硫酸调节pH,用2g/L抗坏血酸替代15g/L抗坏血酸来还原硅钼酸,比色波长由原来700nm调整为680nm,更大地提供了检测灵敏度和准确性。
发明内容
本发明解决的技术问题是,现有技术中对于土壤有效硅的测定方法使用硫酸调节反应前溶液pH,用15g/L抗坏血酸将硅钼酸还原为硅钼蓝,在波长700nm处比色,通过测定蓝色深浅来测定硅浓度,但在实际实验中,发现该法反应显色不明显,测量灵敏度不高。
为解决上述技术问题,本发明所采用的技术方案是,一种土壤中有效硅测定的改进方法,包括以下步骤:
1)试液制备:称取10g左右风干的土样于250ml聚乙烯瓶中,加0.025mol/L柠檬酸溶液100ml,盖好瓶盖,摇匀,于30℃恒温箱中保温5h,取出后干过滤,同时做空白实验;
2)绘制标准曲线:分别准确吸取含硅25mg/L的标准溶液0.00ml、0.50ml、 1.00ml、1.50ml、2.00ml、2.50ml于50ml塑料比色管中,依次加入3.5ml 1mol/L的盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml 2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿比色;
3)样品分析:取试液5-25ml于50ml塑料比色管中,加入3.5ml 1mol/L盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml 2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿,用水做参比,测量吸光度。本法对土壤有效硅检出限为1.2mg/kg,相对标准偏差小于1.7%。
在酸性溶液中,硅酸与钼酸铵生成黄色的硅钼杂多酸,然后以草酸掩蔽磷,用抗坏血酸将其还原为硅钼蓝络合物,其颜色深度与有效硅的浓度成正比,在一定范围内符合朗伯比尔定律,从而可以用比色法进行测定。
进一步地,在上述方案中,步骤1)所述风干的土样经2mm筛孔过筛。
进一步地,在上述方案中,步骤1)所述试液在恒温箱中保温过程中每隔1h摇动一次。
本发明的有益效果是:本发明用盐酸替代硫酸调节pH,用2g/L抗坏血酸替代15g/L抗坏血酸来还原硅钼酸,比色波长由原来700nm调整为680nm,更大地提供了检测灵敏度和准确性。本发明对土壤有效硅检出限为1.2mg/kg,相对标准偏差小于1.7%。
附图说明
图1是硅的标准曲线。
具体实施方式
一种土壤中有效硅测定的改进方法,包括以下步骤:
1)试液制备:称取10g左右通过2mm筛孔的风干的土样于250ml聚乙烯瓶中,加0.025mol/L柠檬酸溶液100ml,盖好瓶盖,摇匀,于30℃恒温箱中保温5h,每隔1h摇动一次,取出后干过滤,同时做空白实验;
2)绘制标准曲线:分别准确吸取含硅25mg/L的标准溶液0.00ml、0.50ml、1.00ml、1.50ml、2.00ml、2.50ml于50ml塑料比色管中,依次加入3.5ml 1mol/L的盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml 2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿比色,见图1;
3)样品分析:取试液5-25ml于50ml塑料比色管中,加入3.5ml 1mol/L盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml 2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿,用水做参比,测量吸光度。
本方法对土壤有效硅检出限为1.2mg/kg,相对标准偏差小于1.7%,具体试验结果见表1。
表1:土壤有效硅测定的精密度和准确度
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明实施例技术方案的精神和范围。
Claims (3)
1.一种土壤中有效硅测定的改进方法,其特征在于,包括以下步骤:
1)试液制备:称取10g左右风干的土样于250ml聚乙烯瓶中,加0.025mol/L柠檬酸溶液100ml,盖好瓶盖,摇匀,于30℃恒温箱中保温一段时间,取出过滤,同时做空白实验;
2)绘制标准曲线:分别准确吸取含硅25mg/L的标准溶液0.00ml、0.50ml、1.00ml、1.50ml、2.00ml、2.50ml于50ml塑料比色管中,依次加入3.5ml1mol/L的盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿比色;
3)样品分析:取试液5-25ml于50ml塑料比色管中,加入3.5ml 1mol/L盐酸溶液,用蒸馏水稀释至25ml,摇匀,加入50g/L钼酸铵2.5ml,摇匀,放置15-20分钟,加入5ml 50g/L草酸,5ml 2g/L抗坏血酸,摇匀,冷却后用蒸馏水稀释至50mL标线,摇匀,放置1.5-2h,于波长680nm处,用1cm玻璃或石英比色皿,用水做参比,测量吸光度。
2.如权利要求1所述的一种土壤中有效硅测定的改进方法,其特征在于,步骤1)所述风干的土样经2mm筛孔过筛。
3.如权利要求1所述的一种土壤中有效硅测定的改进方法,其特征在于,步骤1)所述试液在恒温箱中保温过程中每隔1h摇动一次。
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CN111208118A (zh) * | 2020-03-11 | 2020-05-29 | 内蒙古路易精普检测科技有限公司 | 土壤有效硅的icp测定方法 |
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CN109827918A (zh) * | 2019-04-03 | 2019-05-31 | 广西壮族自治区冶金产品质量检验站 | 掺锡氧化铟粉中硅含量的测定方法 |
CN109827918B (zh) * | 2019-04-03 | 2021-08-13 | 广西壮族自治区冶金产品质量检验站 | 掺锡氧化铟粉中硅含量的测定方法 |
CN111208118A (zh) * | 2020-03-11 | 2020-05-29 | 内蒙古路易精普检测科技有限公司 | 土壤有效硅的icp测定方法 |
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