Method for detecting trace hydroxylamine hydrochloride
A technology of hydroxylamine hydrochloride and a detection method, which is applied in the field of analysis and detection, and can solve the problems of high price, low sensitivity, measurement interference, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0032] The selection of embodiment 1 derivation condition
[0033] (1) Solution preparation
[0034] Hydroxylamine hydrochloride stock solution: Weigh 230mg of hydroxylamine hydrochloride, put it in a 50ml measuring bottle, dissolve it with water and dilute to the mark, shake well to get ready.
[0035] p-Nitrobenzaldehyde stock solution: Weigh 1.25g of p-Nitrobenzaldehyde, put it in a 50ml measuring bottle, add an appropriate amount of methanol, dissolve and dilute to the mark by ultrasonic, shake well, and you get it.
[0036] Sodium carbonate solution I: Weigh 7.4g of anhydrous sodium carbonate, put it in a 50ml measuring bottle, dissolve it with water and dilute to the mark, shake well to obtain.
[0037] Shake the reference substance solution in a water bath at 50°C: Measure 1ml of hydroxylamine hydrochloride stock solution, 1ml of p-nitrobenzaldehyde stock solution, and 0.5ml of sodium carbonate solution I in a 10ml measuring bottle, dilute to the mark with a solvent, s...
Embodiment 2
[0044] Embodiment 2 The setting of chromatographic and mass spectrometry conditions
[0045] (1) Set the chromatographic separation conditions
[0046] The chromatographic column used is Agilent ZORBAX SB-C18, size 150×4.6mm, 5μm; mobile phase A is water, mobile phase B is acetonitrile, gradient elution, flow rate is 1.0ml / min, column temperature is 35°C, injection volume 10 μl; the gradient elution program is:
[0047] time (min) Phase A (%) Phase B (%) 0 70 30 20 20 80 21 70 30 25 70 30
[0048] (2) Set mass spectrometry detection conditions
[0049] The ion source is ESI source, positive ion mode, IS voltage -4500V, air curtain gas 35psi, atomizing gas 60psi, auxiliary gas 50psi, source temperature 500℃, collision gas 9psi;
[0050] Mass Spectrometry Parameters:
[0051] Q1 Q3 DP EP CE CXP 165.1 118.1 -53 -10 -19 -10
Embodiment 3
[0052] The establishment of embodiment 3 standard curve
[0053] (1) Preparation of standard solution
[0054] Hydroxylamine hydrochloride solution: Weigh 15mg of hydroxylamine hydrochloride, put it in a 250ml measuring bottle, dissolve it with water and dilute to the mark, shake well, take 1ml precisely, put it in a 100ml measuring bottle, dilute it with water to the mark, take 1ml precisely, put it in 10ml Bottle, diluted with solvent to the mark, shake well, that is. The solvent is a mixture of methanol and water, wherein the volume ratio of methanol to water is 2:1.
[0055] p-Nitrobenzaldehyde solution: Accurately weigh 33mg of p-nitrobenzaldehyde, put it in a 100ml measuring bottle, dissolve it with methanol and dilute to the mark, accurately measure 1ml, put it in a 10ml measuring bottle, dilute to the mark with solvent, shake well , that is. The solvent is a mixture of methanol and water, wherein the volume ratio of methanol to water is 2:1.
[0056] Sodium carbona...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More