KR20040090356A - The Simplied method of analysis for Nitrate and Nitrite - Google Patents

The Simplied method of analysis for Nitrate and Nitrite Download PDF

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KR20040090356A
KR20040090356A KR1020030024534A KR20030024534A KR20040090356A KR 20040090356 A KR20040090356 A KR 20040090356A KR 1020030024534 A KR1020030024534 A KR 1020030024534A KR 20030024534 A KR20030024534 A KR 20030024534A KR 20040090356 A KR20040090356 A KR 20040090356A
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nitrate
nitrite
analysis
nitrogen
sample
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KR1020030024534A
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Korean (ko)
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전영관
이근헌
한대호
민병섭
전은경
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(주) 휴마스
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/227—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for nitrates or nitrites
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/188—Determining the state of nitrification

Abstract

PURPOSE: A simplified method for analysis of nitrate and nitrite is provided, thereby simply and easily analyzing nitrate and nitrite in the field, and being applied to analysis of nitrate and nitrite in tap water and fresh water. CONSTITUTION: The method for producing powdered reagents for analysis of nitrite comprises mixing powdered reagents consisting of sulfanilamide, N-(1-naphthyl)ethylenediamine dihydro-chloride, hydrochloric acid salt(phosphate salt), with a buffering agent selected from Li2SO4, Na2SO4, K2SO4, MgSO4 or CaSO4 for regulating pH of a sample to pH 2.5 to 3.5. The method for producing powdered reagents for analysis of nitrate comprises mixing powdered reagents consisting of sulfanilamide, N-(1-naphthyl)ethylenediamine dihydro-chloride, hydrochloric acid salt(phosphate salt), a buffering agent selected from Li2SO4, Na2SO4, K2SO4, MgSO4 or CaSO4 for regulating pH of a sample to pH 2.5 to 3.5, cadmium powder and sulfanilic acid. The simplified method for analysis of nitrate and nitrite comprises the steps of: inserting the powdered reagents for analysis of nitrate and nitrite into a vessel to prepare a simplified analysis kit; introducing a sample into the simplified analysis kit; and measuring the color change of the kit.

Description

질산성질소와 아질산성질소의 간이 분석시약 제조법{The Simplied method of analysis for Nitrate and Nitrite}The simplied method of analysis for nitrate and nitrite

우리나라 수질오염공정시험방법에는 질산성질소, 아질산성질소의 측정방법이 잘 설명되어 있다. 이 방법은 여러 가지 약품을 순차적으로 첨가하면서 반응시킨 후 최종적으로 색변화를 관찰하는 것이다.The water pollution process test method in Korea describes the measurement method of nitrate nitrogen and nitrite nitrogen well. In this method, various chemicals are added sequentially, followed by reaction to finally observe the color change.

아질산성질소를 측정하는 방법은 아질산 이온을 슬퍼닐아미드와 반응시켜 디아조화하고 α-나프틸에틸렌디아민을 염산염과 반응시켜 생성된 아조화합물의 홍색을 분석하는 방법이다. 여과한 시료 적당량(아질산성질소로서 약 0.01mg이하 함유)을 취하여 50㎖ 비색관에 넣고 물을 넣어 표선을 채운 다음 슬퍼닐아미드 용액(0.5W/V%) 1㎖를 섞고 5분간 방치한 다음 α-나프틸에틸렌디아민이염산염 용액(0.1W/V%) 1㎖을 넣어 섞고 10-30분간 방치한다, 이 용액의 일부를 층장 10mm 흡수셀에 옮겨 검액으로 한다. 따로 물 50㎖를 취하여 시료의 시험방법에 따라 시험하여 바탕시험액으로한다. 바탕시험액을 대조액으로하여 540nm에서 검액의 흡광도를 측정하고 미리 작성한 검량선으로부터 아질산성질소의 양을 구하여 농도(mg/ℓ)를 산출한다.The method for measuring nitrous nitrite is a method for diazotizing by reacting nitrite ions with a sulfanylamide and analyzing the red color of the azo compound produced by reacting α-naphthylethylenediamine with hydrochloride. Take an appropriate amount of the filtered sample (containing less than about 0.01mg of nitrous acid), put it in a 50ml colorimetric tube, add water, fill the mark, mix 1ml of sulfanylamide solution (0.5W / V%), and leave for 5 minutes. Add 1 ml of α-naphthylethylenediamine dihydrochloride solution (0.1W / V%) and leave for 10-30 minutes. Transfer a portion of this solution to a layered 10mm absorption cell to obtain a sample solution. Separately, 50 ml of water is tested according to the test method of the sample, which is used as the blank test solution. Using the blank test solution as a control, measure the absorbance of the sample at 540 nm, and calculate the concentration (mg / L) from the previously prepared calibration curve.

질산성 질소를 측정하는 방법은 황산산성에서 질산이온이 부루신과 반응하여 생성된 황색화합물의 색을 분석한다. 여과한 시료 적당량 (질산성질소로서 0.01mg 이하 함유)을 취하여 25 ml 비색관에 넣고 물을 넣고 10 ml 로 한 액에 염화나트륨용액(30W/V%) 2 ml를 넣어 섞은 다음 황산 (1+4) 10 ml를 넣어 세게 흔들어 섞고 수냉한다. 여기에 부루신, 술퍼닐산용액 0.5 ml를 넣어 흔들어 섞고 끓는 수욕중에서 정확히 20분간 가열반응시킨 다음 실온까지 수냉하고 물을 넣어 표선을 맞춘다. 이 용액의 일부를 층장 10mm흡수셀에 옮겨 검액으로 한다. 따로 물 10 ml를 취하여 시험방법에 따라 시험하여 바탕 시험액으로 한다. 바탕시험액을 대조액으로 하여 410nm에서 검액의 흡광도를 측정하고 미리 작성한 검량선으로부터 질산성질소의 양을 구하고 농도(mg/l)을 산출한다. 또한 총질소를 분석하는 방법중 질산성질소를 카드뮴 금속을 이용하여 질산이온을 아질산으로 환원시킨후 아질산질소의 양을 구하여 질산성질소를 측정하는 방법도 있다.The method for measuring nitrate nitrogen is to analyze the color of the yellow compound produced by the reaction of nitrate with leucine in sulphate. Take an appropriate amount of the filtered sample (containing 0.01 mg or less of nitric acid), place it in a 25 ml colorimetric tube, add water, and add 2 ml of sodium chloride solution (30 W / V%) to 10 ml of sulfuric acid (1 + 4). ) Mix 10 ml and shake well and cool. Add 0.5 ml of Burucine and Sulfuric Acid solution, shake and mix, heat the reaction for 20 minutes in a boiling water bath, cool to room temperature and add water to adjust the mark. A portion of this solution is transferred to a 10 mm long absorption cell and used as the sample solution. Separately, 10 ml of water is tested according to the test method, and used as the test solution. Using the blank test solution as a control, measure the absorbance of the sample at 410 nm, calculate the amount of nitrogen nitrate from the calibration curve previously prepared, and calculate the concentration (mg / l). In addition, a method of analyzing total nitrogen is to reduce nitrate nitrate to nitrite using cadmium metal, and then measure the amount of nitrite to measure nitrate nitrogen.

이렇게 우리나라 수질오염공정시험방법에 의해 질산성질소 및 아질산성질소를 측정하려면 여러 가지 실험기구를 갖추어야 하기 때문에 현장에서 간단히 측정할 수는 없다.In order to measure nitrogen nitrate and nitrite nitrogen by the water pollution process test method in Korea, it is not possible to measure simply in the field because various experimental instruments should be equipped.

대한민국 특허 출원번호 10-2001-0029824에 의하면 암모니아성, 질산성 및 아질산성 질소를 간편하게 측정할 수 있는 수질조사키트를 개발하였다. 이 방법도 수질오염공정시험방법에 토대를 하여 제작한 것으로 아질산성 질소 측정 시약은 슬퍼닐제(Sulfanilamide)와 유기용매를 포함하는 수용액인 B1시약, N-(1-naphthyl)ethylenediamine dihydrochloride 수용액인 B2시약으로 구성되어 있다.또한 질산성질소 측정시약은 아연과 충진제가 혼합된 C1시약, 슬퍼니산(Sulfanilic acid)수용액인 C2시약, 나프틸디아민 수용액인 C3시약으로 구성되어 있다. 이 방법은 측정시약이 여러 가지 액상 또는 분말시약으로 구성되어 있으며 분석시에는 분석하고자 하는 물에 각 시약을 순차적으로 첨가하게 되어있어 현장에서 간단히 분석하기에는 불편한점이 있다.Korean Patent Application No. 10-2001-0029824 has developed a water quality survey kit that can easily measure ammonia, nitric acid and nitrite nitrogen. This method is also based on the water pollution process test method. The nitrite nitrogen measurement reagent is a B1 reagent, an aqueous solution containing sulfanilamide and an organic solvent, and B2 reagent, an aqueous N- (1-naphthyl) ethylenediamine dihydrochloride solution. In addition, the nitrogen nitrate measurement reagent is composed of a C1 reagent mixed with zinc and a filler, a C2 reagent containing an aqueous solution of sulfanilic acid, and a C3 reagent containing an aqueous naphthyldiamine solution. This method consists of several liquid or powder reagents, and when analyzing, each reagent is sequentially added to the water to be analyzed.

본 발명은 우리나라 수질오염공정시험방법을 토대로 질산성질소, 아질산성질소를 현장에서 간이로 분석할 수 있는 방법을 개발하고자 하였다. 현장에서 다른 기구나 도구를 사용하지 않고 한번의 조작만으로 분석할 수 있게 하기 위하여 혼합분말형태의 시약을 개발하여 밀폐용기에 담은 후 분석하고자 하는 시료를 주입하여 흔드는 것만으로 질산성질소 및 아질산성질소를 분석할 수 있도록 개발하고자 하였다.The present invention was to develop a method for the simple analysis of nitrate nitrogen, nitrite nitrogen in the field based on the water pollution process test method in Korea. In order to be able to analyze in a single operation without using other instruments or tools in the field, we developed a mixed powder type reagent, put it in an airtight container, and then inject and shake the sample to be analyzed. We tried to develop to be able to analyze.

본 발명자들은 우리나라 수질오염공정시험방법에 설명되어 있는 분석방법의 원리를 이용하였다. 분석의 용이성을 높이기 위하여 모든 시약을 분말형태로 혼합하고자 하였다. 분석방법은 용기에 분말상의 분석시약을 넣고 측정하고자 하는 시료를 주입하여 흔들어 혼합한 후 색의 변화를 관찰하여 간이 분석하는 것이다. 혼합된 분말시약을 제조하는 데 가장 중요한 것은 각 분말 시약들간에 반응성이 없어야 하는 것이다. 수질오염공정시험방법에서는 대부분의 약품을 액상으로 사용하고 있는데 이는 측정시료에 주입되는 양을 정확하게 맞추고 또한 반응성을 높이기 위함이라 생각된다.The present inventors used the principle of the analytical method described in the Korean water pollution process test method. In order to increase the ease of analysis, all reagents were mixed in powder form. The analytical method is to put a powdered analytical reagent in the container, inject the sample to be measured, shake and mix, and then observe the color change and perform simple analysis. The most important thing in preparing mixed powder reagents is that there should be no reactivity between each powder reagent. In the water pollution process test method, most of the chemicals are used in the liquid phase, which is thought to be to accurately adjust the amount injected into the sample and to increase the reactivity.

본 발명에서도 아질산성질소를 측정하는 시약으로는 수질오염공정시험방법과 마찬가지로 기본적으로 슬퍼닐아미드(Sulfaniamide)와N-(1-naphthyl)ethylene-diamine dihydrochloride(NED), 염산염이 이용된다. 또한 염산염 대신에 인산염을 사용하기도 한다. 아질산성질소를 측정하기 위하여 홍색의 아조화합물을 생성시키기 위해서는 시료의 페하를 2.5내지 3.5로 조절하는 것이 중요하다. 그러나 분말상으로 조합하였을 때 측정시료의 페하를 조절하는 것은 매우 어렵다. 따라서 본 발명에서는 H2SO4 및 M' SO4를 완충제로 첨가하여 측정시료의 페하가 2.5 내지 3.5로 항상 유지되도록 하였다. 여기서 M은 알카리족으로 Li, Na, K 등이며, M' 은 알카리토류로 Ca, Mg 등이다.In the present invention, as a reagent for measuring nitrous nitrogen, as in the water pollution process test method, basically sulfaniamide, N- (1-naphthyl) ethylene-diamine dihydrochloride (NED), and hydrochloride are used. In addition, phosphate may be used instead of hydrochloride. It is important to adjust the pH of the sample to 2.5 to 3.5 to produce a red azo compound to measure nitrous nitrogen. However, when combined in powder form, it is very difficult to control the pH of the sample. Therefore, in the present invention, H2SO4 and M'SO4 were added as a buffer so that the pH of the measurement sample was always maintained at 2.5 to 3.5. M is an alkali group, Li, Na, K, etc., M 'is an alkaline earth, Ca, Mg, etc.

본 발명에서는 슬퍼닐아미드(Sulfaniamide)와 NED, 염산염, M2SO4 및 M' SO4을 비율에 맞게 혼합하여 아질산성질소 간이분석시약을 제조하였다. 가장 미량 첨가되는 NED의 경우 200메쉬 이하로 미분쇄하였으며 나머지 약품은 구입한 제품 그대로 사용하였다.In the present invention, a mixture of sulphonylamide (Sulfaniamide) and NED, hydrochloride, M2SO4 and M'SO4 in a ratio to prepare a simple nitrite nitrogen assay. In case of the smallest amount of NED, the powder was pulverized to 200 mesh or less, and the remaining drugs were used as they were.

본 발명에서 질산성질소 간이분석시약은 카드뮴 분말을 이용하여 질산이온을 아질산 이온으로 환원시킨후 나머지 분석과정은 아질산성질소 분석시약과 동일하게 이용하였다. 그러나 모든 시약은 하나의 분말로 제조하였다. 질산성질소 간이분석시약에는 카드뮴 분말, 슬퍼닐닉산(Sulfanilic acid), 슬퍼닐아미드(Sulfaniamide)와 NED, 염산염, M2SO4 및 M' SO4이 혼합되어 있다.In the present invention, the simple nitrate nitrogen assay reagent was used to reduce nitrate ions to nitrite ions using cadmium powder, and the rest of the analysis was used in the same manner as the nitrite nitrogen assay reagent. However, all reagents were prepared in one powder. The nitric acid simple assay reagent is a mixture of cadmium powder, sulfanilic acid, sulfanamide, and NED, hydrochloride, M2SO4 and M'SO4.

본 발명을 실시예로 설명하나 실시예에 국한되는 것은 아니다.The present invention is described by way of examples, but is not limited to the examples.

[실시예 1]Example 1

슬퍼닐아미드 : NED : 염산염이 1 : 64 : 0.8이 되도록 하고 측정시료에 첨가하였을 때 페하가 2.5내지 3.5의 범위가 되도록 황산나트륨을 첨가하여 혼합하여 분말상의 아질산성질소 간이분석시약을 제조하였다. 아질산성질소가 0, 0.2, 0,5, 0.8, 1이 되도록 표준액을 제조하였다. 제조된 표준액을 유리 또는 플라스틱 재질의 밀폐용기에 넣고 상기 아질산성질소 간이 분석시약을 넣어 5분후 색의 변화를 관찰하였다. 아질산성질소가 0인 경우 투명한 무색이었으며 아질산성질소 농도가 높아짐에 따라 진한 홍색을 나타내었다.Sulfanylamide: NED: hydrochloride was 1: 64: 0.8 and when added to the measurement sample was added sodium sulfate so that the pH ranges from 2.5 to 3.5 and mixed to prepare a powdery nitrite nitric acid simple assay reagent. Standard solutions were prepared such that nitrous acid nitrogen was 0, 0.2, 0, 5, 0.8, 1. The prepared standard solution was placed in a sealed container made of glass or plastic material, and the nitrite nitrogen simple assay reagent was placed therein, and the color change was observed after 5 minutes. Nitrous nitrite was clear colorless and dark red as nitrite nitrogen concentration increased.

[실시예 2]Example 2

슬퍼닐아미드 : NED : 염산염 : 카드뮴 : 슬퍼닐릭산이 1 : 64 : 0.8 : 2.5 : 0.8이 되도록 하고 측정시료에 첨가하였을 때 페하가 2.5내지 3.5의 범위가 되도록 황산나트륨을 첨가하여 혼합하여 분말상의 질산성질소 간이분석시약을 제조하였다. 질산성질소가 0, 0.5, 1, 5, 10이 되도록 표준액을 제조하였다. 제조된 표준액을 유리 또는 플라스틱 재질의 밀폐용기에 넣고 상기 질산성질소 간이 분석시약을 넣어 5분 후 색의 변화를 관찰하였다. 질산성질소가 0인 경우 투명한 무색이었으며 질산성질소 농도가 높아짐에 따라 진한 홍색을 나타내었다.Sulfanylamide: NED: Hydrochloride: Cadmium: Sulfanylic acid should be 1: 64: 0.8: 2.5: 0.8 and mixed with sodium sulfate so that the pH is in the range of 2.5 to 3.5 when added to the sample. Nitrogen simplified assay reagent was prepared. Standard solutions were prepared such that nitrate nitrogen was 0, 0.5, 1, 5, 10. The prepared standard solution was placed in a sealed container made of glass or plastic material, and the change of color was observed after 5 minutes by adding the simple nitrogen nitrate analysis reagent. When the nitrate was 0, it was transparent and colorless, and became dark red as the concentration of nitrate was increased.

본 발명은 현장에서 매우 간단하고 간편하게 질산성질소 및 아질산성질소를 간이로 분석할 수 있어 현장에서 즉각적인 분석이 가능하다. 또한 본 발명은 먹는 물에도 적용할 수 있어 약숫물이나 수돗물의 간이 검사도 가능하다.The present invention is very simple and simple in the field can be analyzed simply nitrate and nitrite nitrogen can be analyzed immediately in the field. In addition, the present invention can be applied to drinking water, it is also possible to test simple drinking water or tap water.

Claims (4)

질산성 질소 및 아질산성 질소를 간이분석하는데 있어서In the simplified analysis of nitrate and nitrite nitrogen 슬퍼닐아미드(Sulfanilamide), N-(1-naphthyl)ethylenediamine dihydro-chloride , 염산염(또는 인산염)의 3종 분말시약과 측정시료의 페하가 2.5내지 3.5 가 되도록 Li2SO4또는 Na2SO4또는 K2SO4또는 MgSO4또는 CaSO4를 완충제로 첨가한후 혼합하여 제조한 분말상의 아질산성 질소 간이분석시약Li 2 SO 4 or Na 2 SO 4 or Powdered nitrite nitrogen simple assay reagent prepared by adding K 2 SO 4 or MgSO 4 or CaSO 4 as a buffer and then mixing 청구항 1에 있어서 카드뮴분말과 슬퍼닐릭산(Sulfanilic acid)을 추가로 혼합하여 제조한 분말상의 질산성 질소 간이분석시약The powdered nitrate nitrogen simple assay reagent according to claim 1, which is prepared by further mixing cadmium powder and sulfanilic acid. 청구항 1에서 제조한 아질산성 질소 간이분석시약을 기밀용기에 넣고 아질산성 질소를 함유하는 측정시료를 주입한 후 흔들어 혼합하고 소정시간 후에 색변화를 관찰하여 아질산성 질소 농도를 간이 분석하는 방법A method of simply analyzing the nitrite nitrogen concentration by placing the nitrite nitrogen simple assay reagent prepared in claim 1 in an airtight container, injecting a measurement sample containing nitrite nitrogen, shaking the mixture, and observing color change after a predetermined time. 청구항 2에서 제조한 질산성 질소 간이분석시약을 기밀용기에 넣고 질산성 질소를 함유하는 측정시료를 주입한 후 흔들어 혼합하고 소정시간 후에 색변화를 관찰하여 질산성 질소 농도를 간이 분석하는 방법The method for the simple analysis of nitrate nitrogen concentration by placing the nitrate nitrogen simple assay reagent prepared in claim 2 in an airtight container, injecting a measurement sample containing nitrate nitrogen, shaking the mixture, and observing the color change after a predetermined time.
KR1020030024534A 2003-04-17 2003-04-17 The Simplied method of analysis for Nitrate and Nitrite KR20040090356A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100622755B1 (en) * 2004-07-23 2006-09-14 현대자동차주식회사 The analyzing method of the quantity of nitrogen oxide occluded in catalyst
CN100395539C (en) * 2004-11-26 2008-06-18 张山泉 Rapid detecting box for vegetable nitrate content, its detecting reagent and microsampling needle
WO2010141719A2 (en) * 2009-06-03 2010-12-09 University Of Florida Research Foundation Inc. Materials and methods for measuring nitric oxide levels in a biological fluid
KR101145694B1 (en) * 2010-05-24 2012-05-21 주식회사 씨맥 Nitrate concentration measuring method and the measuring kit using thereof
KR101346664B1 (en) * 2012-05-23 2014-01-02 주식회사 씨맥 Nitrate concentration measuring method
KR101346666B1 (en) * 2012-05-23 2014-01-02 주식회사 씨맥 nitrate concentration detecting agent and the kit using thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100622755B1 (en) * 2004-07-23 2006-09-14 현대자동차주식회사 The analyzing method of the quantity of nitrogen oxide occluded in catalyst
CN100395539C (en) * 2004-11-26 2008-06-18 张山泉 Rapid detecting box for vegetable nitrate content, its detecting reagent and microsampling needle
WO2010141719A2 (en) * 2009-06-03 2010-12-09 University Of Florida Research Foundation Inc. Materials and methods for measuring nitric oxide levels in a biological fluid
WO2010141719A3 (en) * 2009-06-03 2011-04-28 University Of Florida Research Foundation Inc. Materials and methods for measuring nitric oxide levels in a biological fluid
US8906693B2 (en) 2009-06-03 2014-12-09 University Of Florida Research Foundation, Inc. Materials and methods for measuring nitric oxide levels in biological fluids
KR101145694B1 (en) * 2010-05-24 2012-05-21 주식회사 씨맥 Nitrate concentration measuring method and the measuring kit using thereof
KR101346664B1 (en) * 2012-05-23 2014-01-02 주식회사 씨맥 Nitrate concentration measuring method
KR101346666B1 (en) * 2012-05-23 2014-01-02 주식회사 씨맥 nitrate concentration detecting agent and the kit using thereof

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