【求助】消毒剂戊二醛的测定方法

为研究戊二醛含量测定新方法,利用高锰酸钾直接氧化戊二醛产生化学发光信号,结合流动注射技术,采用化学发光分析法对戊二醛含量进行了测定.结果,该方法体系的测定线性范围为2.0×10-5～3.0×10-2 g/ml,检出限(3σ)为6.6×10-6 g/ml.对浓度为5.0×10-4 g/ml的戊二醛溶液进行了多次平行测定,相对标准偏差为3.8％.结论,该化学发光法测定戊二醛达到了快速、准确,并成功应用于戊二醛消毒液含量测定

下面的方法但愿对你有用.

Glutaraldehyde Analytical Method

STANDARD PREPARATION

Accurately weigh the 2,4-dinitrophenylhydrazone (2,4 DNP) derivative of the aldehyde to be analyzed into a measured volume of HPLC grade acetonitrile to make a Stock Standard Solution equivalent to 1.0 mg of derivative per ml in acetonitrile. Store the Stock Standard under refrigeration and make fresh monthly. Dilute the Stock Standard Solution in acetonitrile weekly to make 3-5 Working Standards in the range of interest. Store Working Standards in a closed container under refrigeration when not in use. Prior to injection, dilute solution 1:1 with mobile phase, and filter using a 0.45 µm filter.



SAMPLE PREPARATION

Remove each Monitor to be tested from the Return Container. Using forceps or a spatula as a pry, un-snap the Sampling Grid exposing the Sampling Wafer (a single yellow filter disc 3/4" in diameter).



Place the Sampling Wafer into a clean 5 ml glass vial or inert filtration vial (e.g., Whatman Uniprep® Filter Vial, 0.45 µm PVDF, Item No. UN513UAQU). Accurately pipet 1.0 ml of acetonitrile into the vial, close, and seal. Agitate the vial for one minute. Allow the vial to stand 15 minutes, then add 1.0 ml of mobile phase solution, agitate again, and filter the solution through a 0.45 µm filter (or Uniprep). Reserve for HPLC analysis.

BLANK PREPARATION

Remove the Wafer (yellow filter disc) from an unexposed Monitor and process this "BLANK" in exactly the same fashion as the Sample Preparation (above).


HIGH PERFORMANCE LIQUID CHROMATOGRAPHY(HPLC) ANALYSIS

Inject an aliquot of the Sample Preparation from each Monitor to be analyzed into an HPLC System under the following conditions.



HPLC System - Reversed Phase¹ C-18 (15 cm x 3mm id)

Mobile Phase - 50% acetonitrile/50% Acetate Buffer²

(adjust 0.05 M HOAc to pH 5 with KOH in HPLC grade water)

Flow Rate - 1 ml per min (nominal)

Injection Volume - 10-50 microliter (nominal)

Detector Wavelength - 345-365 nm

¹e.g., "Pinnacle TO-11," Restek Corp., Bellefonte, PA
²Conditions given are for formaldehyde. The percentage of acetonitrile may be increased to shorten the elution time for higher aldehydes.

Concomitantly, inject measured aliquots of a BLANK Preparation and three Standard Preparations in the range of interest (i.e. which bracket the concentrations of the Sample Preparations).

CALCULATION


CALCULATION

Determine the Analyte Peak Area as follows:

PEAK AREA (Analyte) =

{ PEAK AREA (Sample Preparation) } - { PEAK AREA(Blank)}



Determine the Analyte Concentration (C) graphically from the PEAK AR versus the Standard Curve prepared by linear regression analysis (least squares).

Calculate Exposure Level from Analyte Concentration as follows.



EXPOSURE LEVEL (ppm) = 1000(C)(V)(F)(R)

(M)(SR)(T)



Where



C = Analyte Concentration Found

(µg/ml Glutaraldehyde di-DNP Derivative)

V = Volume of Solvent (1.0 ml)

F = Fraction of Glutaraldehyde in di-DNP Deriv(0.218)

R = Molar Volume @ 22oC (24.1 l/mole)

M = Analyte Molecular Wt (100.12 g/mole)

SR = Monitor Sampling Rate (ml/min)

T = Sampling Time (min)

EXPOSURE LEVEL (ppm aldehyde) = 1000(C)(V)(F)(R)

(M)(SR)(T)

http://www.instrument.com.cn/show/download/shtml/054289.shtml


这个也许对你有用