CN106290315A - 一种农业肥料中钙的检测方法 - Google Patents
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 45
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000011575 calcium Substances 0.000 title claims abstract description 32
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 30
- 239000013522 chelant Substances 0.000 claims abstract description 34
- 150000005846 sugar alcohols Chemical class 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 13
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 claims abstract description 11
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- 238000000034 method Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000012086 standard solution Substances 0.000 claims description 8
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 3
- 239000001639 calcium acetate Substances 0.000 claims description 3
- 229960005147 calcium acetate Drugs 0.000 claims description 3
- 235000011092 calcium acetate Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- 229930195725 Mannitol Natural products 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000000594 mannitol Substances 0.000 claims description 2
- 235000010355 mannitol Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
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- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000040710 Chela Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229940038879 chelated zinc Drugs 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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Abstract
本发明属于螯合肥料检测技术领域，涉及一种农业肥料中钙的检测方法，先称取两组糖醇螯合肥样品分别加入到离心管中，再在离心管中分别无水乙醇进行水浴加热，使糖醇螯合肥样品充分溶解后室温下放置5分钟，然后将离心管分别放入到离心机中离心两次，取离心得到的沉淀加入蒸馏水搅拌使其溶解得到螯合物溶液并将转移至500ml容量瓶中；再取上清液加入蒸馏水定容到500ml容量瓶中；然后螯合物溶液12.5ml定容到50ml，取上清液8ml定容到100ml，采用ICP‑AES检测法得出螯合物和上清液中钙离子含量，经计算得到钙离子的总含量；其工艺简单，操作方便，原理科学可靠，能准确测定糖醇螯合肥料中螯合钙的含量，实验结果误差小，准确度高。
Description
技术领域：
本发明属于螯合肥料检测技术领域，涉及一种农业肥料中钙的检测方法，特别是一种糖醇螯合肥料中钙的检测方法。
背景技术：
螯合肥料，又称螯合微量元素肥料(chelate micro fertilizers)，简称螯合微肥，是用螯合剂与植物必需的微量元素(硼和钼除外)制成的肥料，目前已有的螯合肥料包括螯合锌、螯合铁、螯合锰和螯合铜等，螯合微量元素肥料比无机微量元素肥料好，在土壤中不易被固定，易溶于水，又不离解，能很好地被植物吸收利用，也可与其他固态或液态肥料混合施用而不发生化学反应，不降低任何肥料的肥效，但由于这种肥料价格昂贵，目前尚未广泛施用。螯合肥料的螯合率的测定研究已在螯合肥料的生产、销售、应用等方面引起了广泛的关注，尽管人们努力提高其螯合效率，改进螯合肥料的检测方法，但基于糖醇为主要螯合剂的糖醇螯合肥料生产及检测行业标准目前仍未推出，现在市场上生产销售的糖醇螯合肥主要采用美国的技术，国内的瓶颈主要根源于尚无螯合元素的有效检测方法，因此，设计一种糖醇螯合肥料中钙的检测方法，对糖醇螯合肥的生产和推广应用具有实质性的作用。
发明内容：
本发明的目的在于克服现有技术存在的缺点，寻求设计提供一种糖醇螯合肥料中钙元素的检测方法，采用EDTA滴定法和ICP-AES检测法(电感耦合等离子体原子发射光谱)进行分析，从而实现钙元素的准确测定。
为了实现上述目的，本发明对糖醇螯合肥中钙元素的检测过程为：
(1)称取4g糖醇螯合肥样品两组分别加入到50ml离心管中， 再在离心管中分别加入40ml无水乙醇，60摄氏度下水浴加热30分钟，使糖醇螯合肥样品充分溶解后室温下放置5分钟，然后将离心管分别放入到离心机中，在4500转/分的条件下离心30min，将离心管中白色物质取出后继续在4500转/分的条件下离心30min，使螯合物完全析出，取上清液和两次离心得到的沉淀分别置于小烧杯中保存备用；
(2)配制20mg/L-80mg/L的钙标准溶液，采用ICP-AES检测法对配制的钙标准溶液生成钙离子标准曲线，取离心得到的沉淀加入200ml蒸馏水，搅拌使沉淀充分溶解得到螯合物溶液并将其转移至500ml容量瓶中；再取上清液加入200ml蒸馏水定容到500ml容量瓶中；
(3)取步骤(2)得到的螯合物溶液12.5ml定容到50ml，取步骤(2)得到的上清液8ml定容到100ml，采用ICP-AES检测法得出螯合物中钙离子含量为m1，上清液中钙离子含量为m2，这样得到钙离子的总含量为m1×40×50×0.001+m2×100×62.5×0.001，实现糖醇螯合肥中钙元素的检测，其中m1，m2单位为mg/L。
本发明所述糖醇螯合钙肥中各组分的重量份为：山梨糖醇5份-10份，甘露醇1份-4份，木糖醇1份-4份，甘油4份-7份，氢氧化钾0份-1份，水35份-45份，乙酸钙4份-6份，硝酸钙80份-95份。
本发明与现有技术相比，其工艺简单，操作方便，原理科学可靠，能准确测定糖醇螯合肥料中螯合钙的含量，实验结果误差小，准确度高。
附图说明：
图1为本发明实施例采用ICP-AES检测法对配制的钙标准溶液生成钙离子标准曲线图。
具体实施方式：
下面通过实施例对本发明做进一步说明。
实施例：
本实施例所采用的糖醇螯合钙肥中各组分的重量份含量为：山梨糖醇5份-10份，甘露醇1份-4份，木糖醇1份-4份，甘油4份-7份，氢氧化钾0份-1份，水35份-45份，乙酸钙4份-6份，硝酸钙80份-95份；所用水均为蒸馏水，pH10的氨-氯化铵缓冲液，所述铬黑T 指示剂是将0.1g铬黑T和10g氯化钠在研钵中充分研磨，保存在棕色瓶中；所述药品均为分析纯，对糖醇螯合肥中钙元素的检测过程为：
(1)样品处理：称取4g糖醇螯合肥样品两组分别加入到50ml离心管中，再在离心管中分别加入40ml无水乙醇，60摄氏度下水浴加热30分钟，使糖醇螯合肥样品充分溶解后室温下放置5分钟，然后将两支离心管分别放入到离心机中，在4500转/分的条件下离心30min，将离心管中白色物质取出后继续在4500转/分的条件下离心30min，使螯合物完全析出，分别取出离心管中的上清液和两次离心得到的沉淀置于小烧杯中保存备用；
(2)配制20mg/L，40mg/L，60mg/L，80mg/L的钙标准溶液，采用ICP-AES检测法对配制的钙标准溶液生成钙离子标准曲线，如图1所示。取其中一个小烧杯中离心得到的沉淀加入200ml蒸馏水，搅拌使螯合物充分溶解得到螯合物溶液并将其转移至500ml容量瓶中；再取上清液加入200ml蒸馏水定容到500ml容量瓶中；
(3)取步骤(2)得到的螯合物溶液12.5ml定容到50ml，取步骤(2)得到的上清液8ml定容到100ml，采用ICP-AES检测法得出螯合物中钙离子含量为m1＝45.15mg，上清液中钙离子含量为m2＝50.37mg，这样得到钙离子的总含量为m1×40×50×0.001+m2×100×62.5×0.001＝90.3+314.81＝405.11mg，其中m1，m2单位为mg/L。
本实施例采用EDTA滴定法对ICP-AES检测法测定的结果进行验证：向另一个小烧杯中的螯合物加入大约100ml水，搅拌使螯合物充分溶解得到螯合物溶液后转移到250ml锥形瓶中，再向锥形瓶中加入pH10的氨-氯化铵缓冲液10ml，保持螯合物溶液的pH稳定在8-10，再加入80mg铬黑T指示剂，摇晃锥形瓶使其充分反应，稳定3min后，用0.02mol/L的EDTA标准溶液进行滴定，溶液由开始的酒红色变为蓝色为滴定终点，然后对钙含量进行计算：钙含量＝CV×0.001/样品中钙离子的摩尔数×100％，其中C为EDTA的浓度，V为消耗EDTA标准溶液的体积，得到螯合物中钙含量为84mg，在误差允许 范围内与ICP-AES检测法测定的结果接近或一致。
Claims (2)
1.一种农业肥料中钙的检测方法，其特征在于其检测过程为：
(1)称取4g糖醇螯合肥样品两组分别加入到50ml离心管中，再在离心管中分别加入40ml无水乙醇，60摄氏度下水浴加热30分钟，使糖醇螯合肥样品充分溶解后室温下放置5分钟，然后将离心管分别放入到离心机中，在4500转/分的条件下离心30min，将离心管中白色物质取出后继续在4500转/分的条件下离心30min，使螯合物完全析出，取上清液和两次离心得到的沉淀分别置于小烧杯中保存备用；
(2)配制20mg/L-80mg/L的钙标准溶液，采用ICP-AES检测法对配制的钙标准溶液生成钙离子标准曲线，取离心得到的沉淀加入200ml蒸馏水，搅拌使沉淀充分溶解得到螯合物溶液并将其转移至500ml容量瓶中；再取上清液加入200ml蒸馏水定容到500ml容量瓶中；
(3)取步骤(2)得到的螯合物溶液12.5ml定容到50ml，取步骤(2)得到的上清液8ml定容到100ml，采用ICP-AES检测法得出螯合物中钙离子含量为m1，上清液中钙离子含量为m2，这样得到钙离子的总含量为m1×40×50×0.001+m2×100×62.5×0.001，实现糖醇螯合肥中钙元素的检测，其中m1，m2单位为mg/L。
2.根据权利要求1所述农业肥料中钙的检测方法，其特征在于所述糖醇螯合钙肥中各组分的重量份为：山梨糖醇5份-10份，甘露醇1份-4份，木糖醇1份-4份，甘油4份-7份，氢氧化钾0份-1份，水35份-45份，乙酸钙4份-6份，硝酸钙80份-95份。
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| CN107311766A (zh) * | 2017-07-24 | 2017-11-03 | 河南捷农生化有限公司 | 一种高含量液体钙肥及其制备方法 |
| CN108675917A (zh) * | 2018-05-17 | 2018-10-19 | 青岛大学 | 一种有机肥料中糖醇螯合钙的分离纯化方法 |
| CN109100312A (zh) * | 2018-07-17 | 2018-12-28 | 青岛大学 | 采用分光光度法测定糖醇螯合钙肥螯合率的方法 |
| CN114573391A (zh) * | 2022-03-01 | 2022-06-03 | 青岛大学 | 一种花生专用糖醇螯合钙肥及其制备方法 |
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| CN107311766A (zh) * | 2017-07-24 | 2017-11-03 | 河南捷农生化有限公司 | 一种高含量液体钙肥及其制备方法 |
| CN108675917A (zh) * | 2018-05-17 | 2018-10-19 | 青岛大学 | 一种有机肥料中糖醇螯合钙的分离纯化方法 |
| CN110015945A (zh) * | 2018-05-17 | 2019-07-16 | 青岛大学 | 一种有机肥料中糖醇螯合钙的分离纯化方法 |
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| CN109100312A (zh) * | 2018-07-17 | 2018-12-28 | 青岛大学 | 采用分光光度法测定糖醇螯合钙肥螯合率的方法 |
| CN109100312B (zh) * | 2018-07-17 | 2019-10-11 | 青岛大学 | 采用分光光度法测定糖醇螯合钙肥螯合率的方法 |
| CN114573391A (zh) * | 2022-03-01 | 2022-06-03 | 青岛大学 | 一种花生专用糖醇螯合钙肥及其制备方法 |
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