EXPERIMENTAL

NOTES PinAAcle 900T AA

AAS-PHARMA Author
Sachin Salunkhe
Application Specialist – Inorganic
Customer Knowledge Centre for Analytical Sciences
PerkinElmer (India) Pvt. Ltd.
Thane – 400 615 India.
Email: application.india@perkinelmer.com

Analysis of Arsenic in Glass using

Hydride generation Atomic
Absorption technique
Abstract
During the manufacturing of glass vials, metal oxides are doped for making special
grade of glasses. Oxides, nitrates and sulfates of arsenic are used as refining agents.
Pharmaceutical glass vials come into direct interaction with pharmaceutical preparations
so it has become a requirement to check the arsenic concentration in glass. This
experimental note demonstrates the analysis methodology to check the total arsenic
content in glass vials which are used in pharmaceutical industries using Perkin Elmer®
PinAAcle 900T AA, FIAS 100 (hydride generation kit) & Anton Paar’s Multiwave 3000,
a Microwave Digestion

Sample preparation
The samples were digested using the Anton Paar’s Multiwave
3000 microwave digestion system equipped with the Rotor
8XF100. Approximately 0.2 g of sample was weighed into the
PTFE-TFM (tetrafluoroethylene, modified) sample vessels to
which added 4 mL HNO3 acid and 4 mL HF acid (all from
Suprapure grade, Merck, Germany. The digestion program used
is given in Table 2. After the digestion sample solutions were
quantitatively transferred in to cleaned polypropylene vials and
all solutions were diluted to 25 mL with ASTM® type I water
Reducing solution (For Arsenic): 5 g each of pure grade
Ascorbic acid was mixed with 5 g of Potassium iodide and
dissolved in 100 mL ASTM® type I water in a polypropylene vessel.
Pre-reduction: 25 mL of sample was taken in 50 mL
polypropylene vessel. 5mL concentrated HCl (suprapure grade)
and 5 mL reducing solution were added into the vessel. The
treated samples were then allowed to stand for 45 minutes.
After prereduction the solutions were diluted to 50 mL with
ASTM® type I water. All calibration standards for arsenic were
prepared in similar way.
0.2% of NaBH4 (used as a reductant) in 0.2% NaOH solution.
10% (v/v) hydrochloric acid was used as carrier solution.
Instrumental conditions Calibrations graph:
Optima TM
8000 DV Optimized Experimental Conditions
Air Flow 7.36 L/min
Acetylene gas flow 1.70 L/min
Read time 20 Sec
Wavelength 193.70nm
Slit width 0.7 nm
Mode AA
Flame Air-Acetylene
Burner head 10 cm single slot
Curve type Linear through Zero
Standards used Standards used 1, 3, 5 µl/L
Lamp Electrode Discharge Lamp
FIAS
Carrier gas flow 75 mL/min
Carrier solution flow 11-12 mL/min
Reductant flow 7-9 mL/min
Sample loop 500 µL
Analytical results & conclusions
The digested samples were analyzed using PinAAcle 900T AAS
and FIAS 100. After verifying the calibration curve by using a
Table 2. Microwave digestion program quality control check standard at the midpoint of calibration,
Step Power (W) Ramp Hold (min) Fan the digested sample were analyzed. The optimized instrumental
(min) parameters are given in Table 1. A spike recovery study was
1 500 10 10 1 carried out at 3.0 µg/L concentration to validate the method
2 1200 10 20 1 developed. The results are given in Table 3.
3 0 -- 15 3
Table 3. Spike Recovery of Arsenic in Glass Sample
P:0.5bar/S, IR:2400C, P:58 Bar
Value obtained Value obtained in Concentration in % recovery
in sample spiked sample solution (µg/g)
solution (µg/L) (µg/L)
0.91 3.80 0.22 96

P:0.5bar/S, IR:2400C, P:58 Bar

Conclusion
The experimental results demonstrated the capability of
PinAAcle 900T AAS and FIAS 100 to analyze trace levels of
arsenic in glass vials. The excellent spike recoveries showed
that the sample preparation protocol followed were excellent.
This also demonstrated the capability of PinAAcle 900T AAS
and FIAS 100 instrument to work in difficult matrices and at
very low concentration levels of arsenic determination.