process control during the manufacture of cosmetics using ... · 4 process control during the...

Introduction

In cosmetics manufacturing, quality control

laboratories are responsible for ensuring

that the necessary and relevant controls

are carried out for sampling and testing per

ISO 22716; ensuring that only materials and

products that conform with the required

acceptance criteria are released for shipment

and use.

The quality control laboratory is expected to

use the available and defined test methods

necessary to confirm that the product

complies with all quality controls and health

and safety regulations.

AN APPLICATION REPORT FROMSPECTRO ANALYTICAL INSTRUMENTS

XRF-90

Effective quality control includes elemental

analysis to be certain that additives or active

reagents are included in the final product in

accordance with specifications. This type of

analysis is not only possible in a main quality

control lab, but can also support production

directly at-line to avoid manufacturing off-

specification products.

SPECTRO XEPOS (XEP05)

Process Control During the Manufacture of Cosmetics Using ED-XRF

Process Control During the Manufacture of Cosmetics 2

Regulations and standards have made it increasingly important for the man-ufacturers of cosmetics to monitor and test the elemental compositions of their products to ensure consumer safety and health. Only materials and products that conform with the respective specifications can be distributed.Quality control laboratories are respon-sible for ensuring that the required testing methods are applied to confirm that the product complies with accep-tance criteria. It is also necessary to use defined test methods to perform the appropriate controls.Energy-dispersive X-ray fluores-cence (ED-XRF) spectrometry has proven itself to be a useful analytical technique for process control. ED-XRF is characterized by relatively simple sample preparation, ease of use and excellent precision. It is, therefore, one of the preferred choices for elemental analysis at-line and in the lab. It can be used to determine the content of additives as well as active ingredients quickly and accurately.This report presents examples for the analysis of color additives in cosmetics and of the active ingredient selenium disulfide in shampoo.

Energy-dispersive X-ray fluorescence (ED-XRF) spectrometry is a useful analytical technique for

process control. ED-XRF is characterized by ease of use as well as precision. Many cosmetics

samples can be non-destructively analyzed with little or no sample preparation. It is, therefore,

one of the preferred choices for elemental analysis at-line and in the lab.

ED-XRF can be used to determine the content of additives as well as active ingredients quickly

and accurately.

Typical color additives, for example, include titanium dioxide TiO2 (21 CFR 732575, CI 77891)

or zinc oxide ZnO (21 CFR 732991, CI 77947). Both are used as pigments or as UV-absorbers in

sunscreen products.

In addition, some active ingredients can also be monitored during production. A typical example

is the analysis of selenium sulfide, which is used as an antifungal agent in shampoos for the

treatment of dandruff and seborrheic dermatitis.

Residues of heavy metals in cosmetics can be dangerous because of their toxicity. Possible

sources of metals in cosmetics can be contamination of basic ingredients, of color additives,

and processing. Therefore, it is also important to monitor the ingredients for cosmetic products

for critical trace elements.

The following report presents examples of the analysis of color additives and selenium disulfide

in shampoo. The screening for heavy metal content in personal healthcare products is described

in a separate application report.


Instrumentation

SPECTRO XEPOS

With its optimized excitation conditions, the SPECTRO XEPOS is well suited to determining the

elemental content of color additives or other ingredients in cosmetics, which can be identified

based on the elemental content of elements in the range of Na-U.

The element range of the SPECTRO XEPOS and

the excitation conditions are given in Table 1.

If elements like cadmium and iodine are of

interest, a fourth measurement condition can be

added to the measurement cycle as well. The

measurement time per sample and excitation

conditions can be optimized depending on the

precision required for the analysis. Typically, a

measurement time in the range of 60 to

300 s per sample is used.

Elementrange kV/mA Excitation

Fe-Nb, Hf-U

40 kV, 0.90 mA

Pd

K-Mn22.5 kV, 2.00 mA

Co

Na-Cl22.5 kV, 2.0 mA

HAPG polarizer

Table 1: Measurement conditions

Applications

Process Control of Color Additives

Table 2 lists examples for color additives in cosmetics and the elements, which can be used to

monitor the additive content during production.

A set of well characterized samples with known TiO2 and ZnO content was analyzed to establish

a calibration covering the typical concentration range.


Color additive CFR CI Element

Bismuth oxychloride 73.2162 CI 77163 Bi, Cl

Iron oxides 73.2250

CI 77489 CI 77491 CI 77492 CI 77499

Fe

Ferric ammonium ferrocyanide 73.2298 CI 77510 Fe

Ferric ferrocyanide 73.2299 CI 77510 Fe

Chromium hydroxide green 73.2326 CI 77289 Cr

Chromium oxide greens 73.2327 CI 77288 Cr

Silver 73.2500 CI 77820 Ag

Titanium dioxide 73.2575 CI 77891 Ti

Aluminum powder 73.2645 CI 77000 Al

Bronze powder 73.2646 CI 77400 Cu, Zn

Copper powder 73.2647 CI 77400 Cu

Ultramarine 73.2725 CI 77007 Na, Al, Si, S

Manganese violet 73.2775 CI 77742 Mn

Zinc oxide 73.2991 CI 77947 Zn

Table 2: Examples for color additives and the elements that can be used to determine their content using ED-XRF

Samples had been prepared in disposable XRF sample cups with an outer diameter of 32 mm.

The analytical side was closed with a 4 µm thick polypropylene film.

The following Figures 1 and 2 show the correlation for TiO2 and ZnO using the SPECTRO XEPOS.

Figure 1: Correlation for TiO2 Figure 2: Correlation for ZnO


Process Control of Active Ingredients Content

Another good example of the benefits of elemental analysis using XRF is the determination of

the content of active ingredients in cosmetics, assuming these can be detected based on the

presence of an element in the range of Na-U.

Typical examples include the process control of content of pyrithione zinc or selenium disulfide

in shampoo.

For products containing selenium disulfide, the analysis

of its content in the shampoo during production is of

interest, as in many countries there are two specifications

available. In the United States, for example, a 1% strength

is available over-the-counter whereas a 2.5% strength is

also available with a prescription.

Figure 3 shows the correlation for Se in shampoo using

SPECTRO XEPOS.

Figure 3: Correlation for Se in shampoo

Summary

This report illustrates the performance of the SPECTRO XEPOS for the analysis of important

elements when processing cosmetics. The screening for heavy metal content in personal

healthcare products is described in a separate application report.

If lab space is limited and a sample changer not required, the SPECTROSCOUT may offer

comparable analytical performance for process control applications.


Choosing an ED-XRF analyzer

ED-XRF technology keeps getting better and better. Today’s most advanced instruments can provide a quantum leap in performance, even over earlier top-ranked models. Look for the following benefits:

High sensitivity and precision. In multi-element analysis of major, minor, and trace element concentra-tions, it’s critical to maximize spectrometric sensitivity and precision. Example: the newest SPECTRO XEPOS analyzers combine exclusive new excitation technol-ogy with innovative detector and tube designs. These help deliver up to 10X greater sensitivity and 3X better precision than previous models. So users get fast, accurate analysis of a wide range of elements, from sodium to uranium.

Long-term stability. Most ED-XRF analyzers shut down their X-ray tube between measurements. Unfor-tunately, resulting temperature variations can nega-tively affect repeatability and accurate readings. To ensure stability, look for an instrument that maintains constant tube power.

Low detection limits. Lower limits of detection (LODs) improve performance with minor and trace element concentrations. The best new models com-bine high sensitivity with minimized backgrounds, achieving exceptionally low LODs for a wide range of elements.

Consumables flexibility. Analysis in an inert-gas environment sometimes produces better results. But constant gas purging becomes expensive. SPECTRO XEPOS instruments offer low-volume helium purging only when required for light elements in liquids and powders, with a vacuum system for solid samples.

Lower costs. Today, an advanced ED-XRF analyzer such as SPECTRO XEPOS exhibits significantly lower costs — of initial investment and long-term owner-ship — than wavelength dispersive X-ray fluorescence (WD-XRF) spectrometers. Yet it generally provides comparable performance for many applications.

GERMANYSPECTRO Analytical Instruments GmbHBoschstrasse 10D-47533 KleveTel: +49.2821.892.0Fax: [email protected]

U.S.A.SPECTRO Analytical Instruments Inc.91 McKee DriveMahwah, NJ 07430Tel: +1.800.548.5809 +1.201.642.3000Fax: [email protected]

CHINAAMETEK Commercial Enterprise (Shanghai) CO., LTD. Part A1, A4 2nd Floor Building No.1 Plot SectionNo.526 Fute 3rd Road East; Pilot Free Trade Zone200131 ShanghaiTel.: +86.21.586.851.11Fax: [email protected]

www.spectro.com

Subsidiaries: uHong Kong: Tel. +852.2976.9162, Fax +852.2976.9132, [email protected], uFRANCE: Tel +33.1.3068.8970, Fax +33.1.3068.8999, [email protected], uGREAT BRITAIN: Tel +44.1162.462.950, Fax +44.1162.740.160, [email protected], uINDIA: Tel +91.22.6196 8200, Fax +91.22.2836 3613, [email protected], uITALY: Tel +39.02.94693.1, Fax +39.02.94693.650, [email protected], uJAPAN: Tel +81.3.6809.2405, Fax +81.3.6809.2410, [email protected], uSOUTH AFRICA: Tel +27.11.979.4241, Fax +27.11.979.3564, [email protected], uSWEDEN: Tel +46.8.5190.6031, Fax+46.8.5190.6034, [email protected]. uSPECTRO operates worldwide and is present in more than 50 countries. For SPECTRO near you, please visit www.spectro.com/worldwide© 2017 AMETEK Inc., all rights reserved, subject to technical modifications • A-17, Rev. 1 • Photos: SPECTRO, Corbis, Getty Images, iStockphoto • Registered trademarks of SPECTRO Analytical Instruments GmbH • : USA (3,645,267); EU (005673694); IR China (0929040); IR Japan (0929040); “SPECTRO”: EU (009693763); IR USA (1080434); IR China (1080434); IR Japan (1080434); IR South Korea (1080434); iCAL: EU (003131919); USA (3,189,726); “SPECTRO XEPOS”: Germany (39851192), USA (2,415,185)

process control during the manufacture of cosmetics using ... · 4 process control during the...

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